Amphetamine Sulphate Synthesis - ‘Reductive Amination using Sodium Borohydride’

> a ketone and an amine > the route via NaBH4/CuCl2

THE Work Up-

>C9H9NO2 MP=63-65°C
>NaBH4 (reducing agent) - Sodium borohydride (somebody say it’s in excess because
it's diprotic. Review the stoiciometry)
>C3H8O IPA – 60,1g/mol – BP:82,5 °C -- d=0.786 g/cm3 solvant polaire miscible dans eau
et alcool de faible masse molaire,
>dH2O
>CuCl2 -134,45g/mol - (oxydant) dichlorure de cuivre attention not to > thats way too much cucl2 for this
reaction, you need a catalytic amount, probably 1 gram for every 10 of nabh4 - The value for copper chloride is
based on anhydrous copper chloride, so make adjustments based on if you're using the dihydrate.Selon Wiki,
on n'utilise le catalyseur que dans une proportion représentant généralement entre 1 et 20 % (en masse ou en
équivalent) par rapport au produits de départ (quantité stochiométrique).
>NaHSO₄ Sodium bisulphate
>NaOH hydroxyde de sodium
>CH2Cl2 DCM 84,93 g/mol (d=1,33g/cm³ - solvent Non Polaire donc non miscible dans l’eau. Miscible dans
acétone, ether et autres solvants)
>MgSO4 Sulfate de magnésium 120,37 g/mol
>AcOH Acetique acide 60 g/mol
>H2SO4 Acide sulfurique 98%
What I do to recrystallize my P2NP -
> Heat some IPA to boiling (2x the amount of P2NP just in case, use even less)
> Put the glass with the P2NP on a hot plate and slowly add IPA while mixing well.
If the solution is not too concentrated (not too much IPA I mean!) the P2NP will start forming its long
needles as soon as the boiling stops.
> After cooling slowly, put the solution in the fridge, then filter the crystals on a Buchner funnel.
> Repeat cooling filtering to get a second crop.
> If you want to get all the P2NP out, you can add a little water to make the IPA cloudy. All crystals will
fall out immediately...

Can be recommend first filtering the catalyst (can be reused several times btw.), wash
catalyst with alcohol, add enough saturated potassium carbonate solution to salt out an
amine/alcohol layer, seperate phases, distill the alcohol off, then directly water-jet-vacuum-
distill the clear colorless product.
By the way, it is in my experience, important to powder the borohydride before really
well, this works much better this way.
Also, I usually use a bit more IPA to get everything well into solution, and fast enough
too.

add grams substance 1 Mol : )

0.1 M 16.3 gr Nitropropene 163.17
0.75 M 28.35 gr * Sodium borohydride 37.8
0.1 M 13..45 gr CuCl2 134.45

> (in 480ml) solvant 1:2 IPA/H2O > can be warmed seperately to 40°C
* can be reduced to 6x mol-eq. / 227 gr NaBH4 per 163 gr p2np (37,8*6=227)

(strong overhead stirring switched on and not shut down till end)

1-phenyl-2-nitropropene (16.3 g, 0.1M) is added in portions to a stirred mixture of

Sodium borohydride (28.35 g, 0.75*M) in 320 ml IPA and 160 ml dH2O, which
increase the temp to 50-60°C.

* Some reports better yield when nitropropene being add in portions and do it fast
to increase the process. Comment said : the complete dissolution of the P2NP
being of utter importance. The solution has to be completely CLEAR no turbidity. If
it does not get clear yor P2NP is dirty.
* Pensez-y. On ajoute de l'eau dans le mélange réactionnel, un mélange
d'isopropanol et d'eau, auquel on ajoute le borohydrure. Donc évidemment, si on
utilise la forme anhydre, elle ne restera pas anhydre. Cela ne devrait pas avoir
d'importance, sauf peut-être de légers effets dus à la modification de la teneur en
H2O, afin d'hydrater et de solvater le CuCl2.
* IPA > You will want to use 15-20 ml/g of either solvent, enough solvent so the
solution turns clear. You should be able to see through the flask and it should not
be cloudy. It sounds like a lot of solvent but trust me, your recovery after cooling
should be around 90%. If you don't add enough solvent to form a clear solution
your crystals will be ugly.
Thereafter a 2M solution of Copper(II) chloride () (50 ml, 0.1M) is added dropwise
causing further heat increase.
The reaction is then held at 80°C for 30 min by extrenal heating, then let cool to
RT.
Boil ?: someone said as hard as possible to drive all shit out. This removes by
steam-distillation all the stuff which steamdistills and is not a salt at this moment
like amphetamine ,
The reaction is quenched with NaOH.

When solution is RT > IPA distill off. - Product steamdistilled rather slowly and not
pushed at all for thats another key to quality.

(sometimes Sodium carbonate and water can be added until no more fizzing (CO2 formation)
because thats much softer on the product and no insane amounts of NaOH needed)

add with stirring 20 ml of 25% NaOH solution to pH 14, and the phases separates
(with amine base in the aquase phase)
now stirring is shut down

The aq phase is extracted 3 x 30 ml DCM.... [patent say IPA], the extracts

combined and dried with MgSO4, then filtered (the amine is a liquid that will
dissolve in most organic solvent).
Distill off solvent yield amine ca 70% (ca 9.5 grams freebase)

Cristallisation-

1:5 IPA and 96% H2SO4 is measured up, put this mix in freezer 15-25 min.
One mol amine freebase (135 gr) is mixed with 375 ml IPA, also put in freezer.

The freebase solution is now placed in an ice bath with stirring at temp 0-10*C, the
acid mix/IPA mix is then slowly dripped in with stirring until pH6, let stir another 30
min, then put in fridge,
filter, re-crystallize with dry acetone to get cleaner product.

9.5 gr freebase. By using the freezer & fridge during crystallization you get 5-10%
more final product. 9.5 gr freebase gives 12 gr sulphate.

==============================================================

Comment :

Quench/Acidify with acetic acid (mixture usually clears up), strip the alcohol
properly - until vapor is 100 C and then keep on distilling a while longer. Switch
receiving flask to a new one. Let mixture cool off and then basify with an alkali
hydroxide, until strongly basic (oily mess will come out of solution). Perhaps add
extra water. Then distill away. When the oil co-distills with the water, inner surface
of glass and condensing liquid will take on a milky appearance. When it's not milky
any longer, keep distilling (perhaps 30-60 minutes?). Hopefully you will now have a
reciving flask with an upper layer of oil. Pour entire contents of receiving flask in a
sep funnel. You can separate the distinct oil layer first if you want to, but either way
you should extract 3 times with for example iPrOH or toluene. You might want to
add some KOH/NaOH and/or brine, if using iPrOH you definitely should do that.
The combined organic phases are dried (for example with MgSO4) and the drying
agent filtered off into a dry flask.

Put that flask in the freezer until decently cold. Put it into an ice bath and put it on
a stirrer with a stir bar in the flask. Add concentrated sulfuric acid, dropwise with
good stirring. Sulfate salt should be very evident within a short amount of time
after adding the first few drops. Measure the pH as often as you need *use pre-
wetted pH-paper*, but naturally more often as the pH approaches neutrality. *Don't
overshoot!* Even just one drop too many of conc. H2SO4 can mess it up pretty
badly, IME a thick paste can become a loose slurry that is not overly filterable.
Filter off your salt, wash with acetone and then a dash of DCM. Let it all dry in a
pyrex dish or similar, then crush lumps up and let it dry more. Voilá!

==============================================================

=FROM Vespiary

I would recommend to get used to the process and take like 5-10ml of the
freebase, dissolve that in 10x acetone and add a 10% H2SO4 in IPA solution to it,
very slowly due to it heating up of course, and and especially slowly in the end
when you have almost reached neutrality.
Amphetamine sulfate does not form instantly, so it can happen that you measure a
pH of 7, but two minutes later when you measure again, you see it is now acidic
and not neutral anymore.
Because of this, be especially slow when you get near this point.
But you should also put a little bit of the freebase in acetone away, to correct the
pH if you overshoot on acid and need to readjust to a higher pH.

Amphetamine sulfate is typically precipitated from an alcohol solution of the base

using H2SO4. If you save the filtrate and alcohol washings and later distill off the
alcohol you'll find you get some amphetamine sulfate which can be purified by A/B
extraction and vacuum (or even 1 atm) distillation of the free base. If you used the
Leukart reaction on P2P you might find the amphetamine sulfate in the filtrate to
have the consistancy of peanut butter, but the (first) ppt. is white. After washing
with alcohol and then made into a block to dry, a brown coloring forms on it which
can be scraped off and the blocks stay white. Also, I know of someone who tried
recrystallizing about 30 grams of amphetamine sulfate from water, but after
concentrating and cooling the filtrate several times to get more ppt. until there was
no water left he found that about 3 grams disappeared which must have
evaporated with the water, so he decided to stick with ppt. from alcohol using
 H2SO4, wash with alcohol, make into blocks, scrape off color after drying and also
saving the alcohol filtrate to recover a small amount (5%?) of the amphetamine
sulfate.

Also, if you add too much H2SO4 to amphetamine base in alcohol the sulfate
redissolves, so its best to add small amounts of H2SO4 at time, filter, then add
H2SO4 to the filtrate to get more ppt., filter and repeat until there's no more ppt.
Save the alcohol filtrate from several runs to get more amphetamine sulfate as
described above.

Abstract-

The workup - is carried out else too, borohydride is quenched with AcOH
as usual, IPA distilled off then, base added, so any copper complex is broken and it
allows for simple steam distillation then to isolate the amine directly from the reaction
flask.
I always re-distill the amine freebase to get ultra clean product +99%, without re-
distillation of amine oil you get 90-93% final roduct which has the familiar unpleasant
side effects like drier mouth, face tics, jaw clenching, lower sexuality, erection problems
etc

The first is using sodium borohydride plus transition metal salts (nickel
chloride or copper chloride). Usually, on its own, NaBH4 will only break the double bond
on a nitroalkane, forming dihydro-P2NP or dihydro-nitrostyrene. However, if you do the
reaction with the addition of a transition metal salt as a catalyst, the resulting borate
(liberated from the borohydride by water) will displace the chloride ion, yielding nickel or
copper borate, which increases its oxidative state and therefore acts as an electron
donor (thus it can donate more electrons to a substrate present in the solution). In the
presence of nitrostyrene or P2NP this means it can completely reduce the whole thing
in a one-step, thirty minute reaction to phenethylamine or amphetamine, requiring a
relatively very small workup and time investment (compared to zinc/hcl). Yields are also
pretty high, up to around 60-70 percent for ring-substituted nitrostyrenes (not as high as
the reported 80-95% yields from zinc/hcl but still very good).

This valuable method, especially for nitropropenes. It has been tried by several
people on 1-phenyl-2-nitropropene, with high success in 80-90% direct amine
yield. Some report yields of +90%. Usually the use of NaBH4 has been 6 to 6.5
mol-eq.

I can confirm from own experiments, that it is indeed possible to reduce a

nitropropene into yields of above 80%.
The reaction is done more harsh, as the nitropropene stands much better to be
added fast enough to cause the reaction being at constant reflux during this, and it
even proved to increase yield.
https://www.thevespiary.org/rhodium/Rhodium/Vespiary/talk/
index.php/topic%2C3519.0.html

https://www.sciencemadness.org/talk/viewthread.php?
tid=4965

Another short workup - from thevespiary forum usefull to see the proportion
of our exploited chemicals

"With vigorous stirring, to 5ml of IPA / 1g of P2NP and 0.4 times volume of H2O
in RBF was dumped 6 mol eq. of NaBH4.

Recrystallized P2NP was washed with sodium bisulfite solution***, then with and
water and it was then added in small portions to the mixture to minimize frothing.
No external cooling applied. After all substrate was added and near-colourless
solution is obtained, the solution left stirring for 30 minutes. Claisen adapter was
fitted to the rbf with reflux setup and addition funnel. With one portion, 10%-mol
equivalent (for the nitroalkene) of CuCl2.2H2O dissolved in IPA was added to the
solution via the funnel. It was refluxed for 30 minutes.

After which the remaining NaBH4 was destroyed by adding about 50% acetic
acid untill the fizzing stopped and the solution was fairly acidic.

Lors de la dernière réaction, j'ai ajouté de l'acide acétique pur et après

quelques minutes d'agitation, la solution est devenue d'une belle couleur
bleu coolaid et a semblé dissoudre le cuivre2.Est-ce que le fait d'en ajouter
trop est contre-productif ?I always just add a random amount most Likely
very much over kill just so I know everything g is acidic before I strip IPA.

***I wash the nitropropene with sodium bisulfite solution to get rid of unreacted
benzaldehyde. Maybe crashing the nitroalkene into bisulfite solution would be better,
then recrystallization... Anyway then I rinse the crystals with ice cold water (either by
dumping them into water and then filtering or just on the buchner) and suck to
somewhat dryness.

With the claisen adapter still attaced, short path distillation setup was rigged and
everything below 100'C was stripped. Then the solution was made basic dripping
strong NaOH solution to the reaction flask and steam distilled. Additional very
dilute NaOH solution was added through the addition funnel every now and then.
The distillate was then made slightly acidic with H2SO4 and evaporated. Total
yield after recrystallization: 80% mol wise from the P2NP due to very sloppy work"

////// Une autre question que j'ai en ajoutant du h2so4 au H2O et à la base
d'amphétamine, je comprends qu'on peut suracidifier et dire que si la base est
dans un solvant comme le toluène, le sulfate d'amphétamine se dissoudra à
nouveau dans la solution. Est-il possible de le sauver quand cela se produit ? Je
pense qu'il suffit d'ajouter du NaOH et de le transformer en base libre à nouveau,
mais quand cela se produit, il semble que je perde tout et que je ne puisse pas
récupérer l'amph. Encore une fois.

Qu'arrive-t-il à l'amph quand on ajoute trop de h2so4 ? Pourquoi se redissout-il ?

Comment peut-on sauver l'amph. Quand cela arrive ?
>>> For quenching the borohydride, when done at a 10mmol scale, it only took
a few drops of 50% v/v AcOH to quench, there seems to be very little left over,
once the borohydride has first reduced the nitroalkene to nitroalkane and then
reduced the CuCl2 to Cu(0).
Quench of the borohydride wasn't violent at all, slight fizzing when adding the
AcOH (as either 25 or 50%, forgot which, aqueous) dropwise, just a bit of
hydrogen evolution, one can tell when the NaBH4 is quenched by the way that
after it has, adding the acid dropwise, H2 evolution takes place with each drop,
until one drop after the last one required to decompose the remaining NaBH4
traces, which, as it's all quenched, will not induce any further fizzing or bubbling,
since it's all done. Using the bubbling of H2 during the quench, and dropwise
adding 50% or 25% AcOH allows it to bee precise, to within a single additional
drop of acid.

>>> suggestions sur la façon de réduire en poudre le NaBH4 ? Il suffit de le mettre

au milieu d'un morceau de sac plastique et de l'écraser avec le fond d'une tasse à
café ou toute autre surface plate d'un objet qui ne se brisera pas sous la pression,
puis d'utiliser le côté de la tasse pour le rouler d'avant en arrière. La stabilité à
l'air/sensibilité à l'humidité du NaBH4 n'est vraiment pas un problème.
Le mien se présente généralement sous une forme plutôt poudreuse, avec tout au
plus quelques grumeaux pas très durs, et ceux-ci peuvent très simplement être
réduits en poudre en les écrasant avec une spatule ou une cuillère plus grande...
pas en une poudre fine, semblable à de la poussière, ce n'est pas nécessaire, il
suffit de se débarrasser des grumeaux les plus gros pour moi.
Je sais que l'ancien borohydrure peut former des masses dures avec de gros
grumeaux…
Je n'ai encore rien trouvé qui puisse indiquer que ce n'est pas conseillé pour le
borohydrure de sodium...
Le sac ici n'est bien sûr pas si important pour être étanche, mais je déconseille le
papier car le NaBH4 est un peu hygroscopique et colle au papier s'il y est laissé
trop longtemps, et certainement plus vite s'il est en poudre.
De plus, je m'attendrais à ce que le borohydrure perde un peu de pouvoir
réducteur quand il est vraiment fin, je ne sais pas, mais ça n'aurait pas beaucoup
d'importance de toute façon.
>>>

------------------------------------------------------------------------------------------------------
>>> It's been done with 500g of P2NP using 10L RBF and refluxing for 2 hours,
90% yield. Adding everything (near) refluxing temperature increase yield.
I use 5ml IPA and 2.5ml H2O for every gram of P2NP I use.
After extremely slow addition of P2NP to minimize frothing and after it is all added
I let this react with vigorous stirring for 30-45 min.

I'll then attach a reflux condenser and add in all at once/or in 2-3 additions an
IPA/H2O solution of my home made very light blue in color CuCl2 . (10% mol eq.
For P2NP)
So for every gram of P2NP I use .1g of CuCl2.
When I add this the reaction mix instantly turns black and heats up.
I'll then reflux this for a good 30-45min

After I let reflux I'll add to reaction mixture through reflux condenser (while still hot)
Glacial Acetic Acid untill fizzing stops and mixture is very acidic. (Usually I add a
large excess of GAA)
After I add GAA, shortly after the reaction mixture takes on a very blue transparent
color. Exactly like blue coolaid.
When I stop stirring two blue transparent layers form in the flask and a small
amount of black precipitate sits on the bottom.

I'll then set up for distillation and distill off everything below 100c.
Once temp reaches 100c I'll switch the receiving flask. I'll then add very strong
NaOH/H2O (I don't usually make a specific NaOH/h20 % solution , I basically just
add a large amount of NaOH to a beaker and add water and mix untill it dissolves)
I then add this to reaction flask.
I then collect H2O/freebase oil in receiving flask.
Usually the H2O/freebase mixture in the receiving flask is a milky white solution
with small amounts of clear oil floating on top.

Once the water distillling over becomes clear I stop distillation.

I now drip in 2 drops (I don't have any PH paper at the moment) of
phenolphthalein solution into the freebase and water mixture turning it purple/pink.
Now I'll drip in diluted H2SO4 until the pink color disappears and I don't see any
freebase oil floating on top of the water.

I now place the solution in a beaker on the hot plate with a stir bar and boil down
to dryness with stirring.
I am then usually left with a whitish substance caked to bottom of the beaker to
which I'll add acetone and boil with mixing for around 1 minute
Then I filter through a coffee filter and collect amphetamine sulphate and let
residual acetone evaporate.

I'm always left with a shitty yeild and don't understand why. I think next time after
distilling off IPA I'll basify the reaction mix and then extract freebase with DCM. I'll
then separate/collect DCM, dry with MgSO4 and then evaporate off DCM leaving
me with just the freebase oil. I'll then know exactly how much I have and then I can
add the exact amount of H2SO4 need to convert it into the sulphate.
-------------------------------------------------------------------------------------------------------------

------------------------------------------------------------------------------------

Best results regarding yields and (more important in my eyes) quality were achieved by:

- Al into the flask (shavings, 99,9%)

- IPA, acetic acid, water, warmed seperately to 40°C and P2NP dissolved. The complete
dissolution of the P2NP being of utter importance*. Then HgCl2 (nitrate will work fine
too) added and dissolved. Stirring of course, what else.
- This dumped onto the Al.
- Strong overhead stirring switched on and not shut down till end.

And here we go, refluxed with heating for 6 hours after the wild part was over.

- Water added and alcohol distilled from solution

- Water distilled from solution - not all but a good part of it. Boil it as hard as possible to
drive all shit out.
This removes by steam-distillation all the stuff which steamdistills and is not a salt at this
moment like amphetamine.
- Sodium carbonate and water added until no more fizzing (CO2 formation)**. NaOH 10%
solution (cold) added to ph 14.
- Product steamdistilled rather slowly and not pushed at all for thats another key to quality.
Now stirring is shut down.
- Collected in petrolether, filtered, separated and solvent switched to IPA (Petrol ether
distilled mostly out, IPA added, rest ether and some IPA distilled out) This takes no time at
all***.
This removes all water too. Salt formation is superior in alcohols though.
- H2SO4 well mixed with the 5-fold amount of IPA is slowly added, fridge, filtration and
again until no more clouds form and it starts turning pink. Washed with small amount of
dry acetone or better ethylacetate.

* the solution has to be completely CLEAR no turbidity. If it does not get clear yor P2NP
is dirty.
** thats much softer on the product and no insane amounts of NaOH or KOH are needed.
 *** petrol ether is superior in selectivity on extraction but a beast to make the salt in.

The result is something what does already optically only remotely resemble the pictures of
horrible unclean, smeary discolored and revolving smelling shit one sees posted or is told
on boards, in pdfs (Oparaya's for example), or at trading places (yellow! yellow P2NP
stains declared as a sign of quality! Vomit!).

I know everything about this "almost amph" as it was what was produced in the beginning,
in all known (and some new) variations.
Most simply declare dirt to gold and thats that.
A few work on though.

Oh! On the boards EVERYONE is only after highest purity.

That is one of the more funny parts of the game here....
...just dont buy it.

your choice.

/ORG

Is amphetamine soluble in water?

They are weakly basic substances and can exist as either in a free base form or react
with various acids to form salts such as amphetamine hydrochloride. The salt forms of
t the amphetamines are highly water-soluble whereas the free base forms are less
so

Other Experimental Properties

Colored liquid with an amine odor
Volatilizes slowly at room temp

- Crystals > bitter taste; sinters at about 150 °C; decomposes around 300 °C; pH of
10% solution is about 4.6. More soluble in water than amphetamine sulfate; slightly
soluble in alcohol; practically insoluble in benzene, chloroform, ether /Amphetamine
phosphate/
- Crystals > slightly bitter taste followed by sensation of numbness; MP above 300 °C
(decomposes); solution of 1 g/10 mL water has pH 5-6; 1 part dissolves in 8.8 parts
water, 515 parts 95% alcohol/amp sulfate

https://pubchem.ncbi.nlm.nih.gov/source/hsdb/3287#section=Human-Toxicity-Excerpts-(Complete)
https://pubchem.ncbi.nlm.nih.gov/compound/Amphetamine

https://www.thevespiary.org/rhodium/Rhodium/Vespiary/talk/index.php/topic%2C3701.0.html

About The Ingredients And Procedures-

CuCl2

The Cucl2 + NaBH4 method is superior, best of all p2np reduction I've ever done,
but only up to 20 gr batches, the more you increase Mol per batch the lower
theoretical yield you'll have (all people I know say the same., so I would be very
suprized if someone have other news to tell) . The sodium bisulphite washings of
the p2np is first time I see someone mention here (THUMBS UP), that superb,
very important to have good yield for whatever you're using your p2np. That's the
far best way to clean out all benzaldehyde contamination of the p2np, and
whatever reaction you wanna do with your p2np the benzaldehyde is a bitch and
will interfere and gives lower yield ketone, oxime, nitroalkane or amine. Always
wash p2np with sodium bisulphite solution and recrystalize before doing any
reaction A/B.

Is CU acidic or basic?
However, copper, and most transition metals, often exist as positively charged ions
in solution. Positive ions are electron pair acceptors, and can be considered Lewis
acids. To reiterate, copper atoms themselves are not acidic or basic, but copper
ions are acidic.

Preparation CuCl2 solution

Le catalyseur, qui est généralement en quantité bien plus faible que les réactifs,
n'est pas consommé et est retrouvé inchangé à la fin de la réaction. S'il est
séparable aisément du milieu réactionnel, il pourra être recyclé dans une nouvelle
synthèse.
Copper(II) chloride dihydrate is a beautiful green crystalline solid, while its diluted
aqueous solution has a pale blue colour
Molarity = number of moles of solute /volume of solution in litre
Molarity = mass of solute (in grams) /molecular mass x volume of solution in litre
2M = le nb de moles de soluté dissout dans 1L (1dm3).
If 2 moles of a solute are present in one litre of a solution then the molarity of
solution will be (2M).
C=n/V

2M signifie qu’il doit y avoir 2 moles de soluté présent par L de solution soit:
2*134,5=269g/L (ratio 0,1M=26,9g/L). Il doit y avoir 26,9g/L au total.
on veux réaliser 50ml (sachant que 1 litre = 10dl = 100cl = 1000ml = 1kg =
1000g)
26,9g > 1000mL
x > 50mL
Puis, x=50*26,9/1000=1,345g de CuCl2 dans une solution de 50 ml.

Explanation:
To make x mL of 2M CuCl2 solution, you need to make sure that every litre of the
solution contains 2.00 mol.
So, 1 L of 2M CuCl2 solution contains 2×(134,5) g=269g CuCl 2

If we mix 40.0 g of NaOH with enough distilled water to make 500 mL, we will get
a 2.00 M NaOH solution.

In what volume of the solution?

1 L X 2 M X 13,45 g/mol = x g NaOH in 1 L of 2M solution

To calculate the mass in any other volume, just replace the “1L” in the calculation
with any other volume (in L).

Pour une Concentration de 0,1M avec masse molaire de 134,45g/mol

.48 g/mol. 1/10th of 170.48 g is 17.048 g, so this is the amount of the CuCl2*2H20
you need for the solution you are tryin
A 100ml 1M CuCl2 – H2O SOLUTION
Firstly, 100 ml at 1M is 1/10th of a mole of Copper chloride dihydrate. Knowing
this, you must portion out 1/10th of a mole of CuCl2 *2H20 and in order to do this,
you also need to know its molar mass; it happens to be 170.48 g/mol. 1/10th of
170.48 g is 17.048 g, so this is the amount of the CuCl2*2H20 you need for the
solution you are trying to make. Since you need 100 mL of the solution, it is
important that you put the CuCl2*2H20 in the volumetric flask (technically you can
use any container, but volumetric flasks are very accurate) first and then pour in
the water to the 100 mL line. If you put 100 mL of water in first and then add the
CuCl2*2H20, it will result in a solution that is more than 100 mL, which will in turn
have a molarity that is not quite 1M. Always add the solute before the solvent. In
short, to make x mL at y M for any solution, multiply x by y and multiply that by the
molar mass of the solute. Add solvent to that mass of solute until you reach the
desired volume

.48 g/mol. 1/10th of 170.48 g is 17.048 g, so this is the amount of the CuCl2*2H20
you need for the solution you are tryin

The purpose of this experiment is to acquaint you with the concept of

concentration of solutions. Although there are a variety of ways of describing a
solution’s concentration, we will use just one system in this experiment, that of
“molarity,” or
“moles per liter,” abbreviated mol/L or M. The experiment will also give you a
chance to see how differences in concentration affect the behavior of a solution,
making it react faster or slower, and making it able to react with more or less of
some other substance
(for the same volume of solution).
“Prepare a tenth of a liter (0.10 L) of a 1 M solution of CuCl2•2H2O.” What,
exactly, does this statement mean? First of all, a tenth of a liter needs to be
expressed as a certain number of milliliters, since our laboratory graduated
cylinders are marked off in milliliters. You will be making, then, 100 mL of solution.
What does the “1 M” mean? It means one mole of the material that you are going
to dissolve – in this case, CuCl2•2H2O – would be present in one liter of a solution
that has the concentration described as “1 M.” (M really says, “moles of dissolved
material per liter of solution.”) However, we will not need a full liter, so we will make
only 0.10 L (100 mL). Question: If you need 170.05 grams (which is one mole of
CuCl2•2H2O) to make one liter of 1 M solution, then how much will you need to
make just one-tenth as much solution? grams, or moles
Sodium Bisulfate is an acidic salt (acidic solution is produced after salt is
dissolved in a solvent)which is produced by partial neutralization of Sulfuric acid
(H2SO4)with an equivalent amount of sodium base, basically in the form of sodium
hydroxide (NaOH) or sodium chloride (NaCl). The anhydrous is being hygroscopic
in nature. The solutions of Sodium Bisulfate are acidic in nature with a pH value of
1 for every 1M solution. It is a white and relatively dry granulated compound. It is
corrosive to metals and tissues and also is soluble in water.
Physical Properties: Sodium Bisulfate of NaHSO4 is usually accessible in both
monohydrate (hydrate comprising of one mole of water/mole of the compound),
NaHSO4.H2O and anhydrous (dry) forms. Anhydrous NaHSO4 is a dry granulated
white powder, having a density of 2.74 g/ml with a melting point of 315 °C.
Whereas, monohydrate is a white colored granulated solid having density of 1.8
g/ml with a melting point of 59 °C. Monohydrate is considered a dry acid which is
appropriate for safe storage and shipping. Its water solubility is 28.5 g/100 ml (25
°C) and 100 g/100 ml (100 °C) respectively
 DROP IDEAS

Amines and amides are very weak acids and only react with very strong bases.

Comment identifier la phase aqueuse de la phase organique ?

En cas de doute pour identifier les phases, on peut prélever avec une pipette
quelques gouttes de la phase à identifier et les ajouter dans un tube à essais
contenant un peu d'eau : si elles se mélangent il s'agit de la phase aqueuse, si
elles forment une nouvelle phase il s'agit de la phase organique.

On sait que la masse volumique de l'eau est : ρ eau = 1 000 g/L = 1 kg/L. Car
l’eau est une constante étalon est a une densité de 1.
 BASIC THEORY

An acid is a compound that releases H+ ions into a solution. So that there is more
H+ than HO- ions.

A base is a compound that can react with H+ ions to neutralize them and form a
salt. Bases come with a huge variety of cations (positively charged ions) and
anions (negatively charged ions). In base we can resume there is more HO- than
H+.

An example of an acid reacting with a base is hydrogen chloride (HCl; an acid)

and sodium hydroxide (NaOH; a base). When these two react the products are
water and sodium chloride.

Common acids are nitric acid, hydrochloric acid (HCl in water), sulfuric acid,
formic/acetic/benzoic/other organic acid(s), and phosphoric acid. Of these, sulfuric
acid is the strongest.

Acids are also often oxidizing in nature, though not always. Sulfuric acid and nitric
acid are both oxidizing acids (nitric is very oxidizing), while the organic acids
(excluding formic acid) and phosphoric acid are all very neutral towards redox. HCl
is extremely weakly reducing, with the heavier halogen acids (hydrogen iodide and
hydrogen bromide) being more reducing; formic acid, oxalic acid, and sulfurous
acid are all quite reducing.

Common bases include hydroxides (the cation is fairly irrelevant), (bi)carbonates,

and ammonia (and related amines; this is a lewis base and will be covered more in
a later lesson).

The strength of bases is limited by the solvent being used. For example, the
strongest base that water can support is a hydroxide. This is because water is
slightly acidic and any base stronger than a hydroxide will react with the water to
form a salt (a hydroxide). Liquid ammonia can handle stronger bases as ammonia
is much less acidic than water (water's pka is 14-16 while ammonia is >30).

General bases are sodium hydroxide, potassium hydroxide, and calcium

hydroxide. These bases are the most common and least reactive, and are non-
toxic as salts (to a degree; never ingest a solution that does not have a PH
between 4 and 9, your body is not built for that type of abuse). Other weaker
bases that are common for general use are (bi)carbonates and phosphate salts.
These last bases are useful for making buffer solutions or destroying acids
(basically just a buffer solution) more than actually making a solution basic.
Stronger bases will need to be made, and the strongest base that you will likely
have access to is Grignard reagents (magnesium is cheap enough that using
these is not extremely wasteful as long as it is a valuable reaction). It is possible to
make bases like N-butyl lithium (!), but it is very dangerous (making and using)
while only offering a few advantages.

Acids are also often oxidizing in nature, though not always. Sulfuric acid and
nitric acid are both oxidizing acids (nitric is very oxidizing), while the organic acids
(excluding formic acid) and phosphoric acid are all very neutral towards redox. HCl
is extremely weakly reducing, with the heavier halogen acids (hydrogen iodide and
hydrogen bromide) being more reducing; formic acid, oxalic acid, and sulfurous
acid are all quite reducing.

C Polar compounds dissolve well with Polar solvants. In the same manner Non
Polar compounds dissolve in Non Polar solvants. Therefore if a compound and a
solvant have identiques properties they dissolve well and are miscible.

If we try to mix NP/P there is no sulubility or miscibility. The more dense (d) or thick
will leave at the bottom and d<1.

We use solvants in reactions to mix the reageants together and make them react.
Dans une réaction chimique exothermique, l'énergie dégagée par la formation des
liaisons chimiques dans les produits de réaction est supérieure à l'énergie requise
pour briser les liaisons dans les réactifs.
De nombreuses réactions impliquant des acides ou des bases sont
exothermiques.

SOLVANTS
Polar solvant

P2NP Preparation

Après la filtration par système buchner vous obtiendrez peut etre une pate
jaune gorgée de solvant. Un bon moyen de nettoyer celui-ci est de
commencer par le faire sécher puis des les dissoudre à nouveau dans un
faible volume d'alcool isopropylique chauffé. Et maintenir le tout à haute
température au bain marie. Quand tous les cristaux sont dissouts mettre une
coupelle ou un film d'aluminium sur l'orifice du récipient peut s'apéréer utile
pour éviter trop d'évaporation. Remettez le récipient au freezer et attendez
l'apparition des cristaux. Et repetez l'étape du filtre buchner en nettoyant
avec de l'eau pure. Faites secher et vous récuperez des cristaux jaune pale
Produits à prévoir
80 mL Toluene (ACS)
40 mL Benzaldehyde (~99%)
30 mL Nitroethane (>99%)
10 mL n-Butylamine (p.a.)
Procédure
Les produits sont tous mélangés dans le toluène dans un ballon de 250ml,
des pierres d'ébullition (boiling stones) sont ajoutée et le Dean&Stark est
monté (piège de 10ml) ainsi qu'un condenseur. L'objectif est de porter la
solution à ébullition pour que que tout coule nettement depuis la surface du
condenseur.
Après 1h, 2.7ml d'eau se trouvaient dans le piège. Après 6h c'est environ
7.0ml qui s'y trouvent soit environ 100% de l'eau en théorie (cela s'est peut
etre passé 30min plus tôt, le chimiste faisait une petite sieste). La solution
est vidée dans un bécher de 250ml et est refroidi à température ambiante.
Quelques cristaux de phenyl-nitroporpène apparaissent. La solution est
ensuite refroidie doucement à -10°C au freezer. De beaux cristaux
apparaissent et il ne semble pas nécessaire de purifier (35g de cristal
récupéré avec un filtre). Il peut sembler nécessaire d'utiliser une filtre
buchner pour aider la filtration à la sortie du freezer. Agissez rapidement,
quand la température augmentera certains cristaux se dissolveront à
nouveau et pourront etre perdus à travers le filtre. Le filtrat est concentré
sous pression faible et refroidit comme ci-dessus. Les cristaux sales tombent
et sont recristallisés avec 50ml de MeOH ou d'alcool isopropylique (6g
récupérés) Au total 41g de P2NP sont récupéré (64%).