Chapter Fourteen

HI Want Some Methylamine!"

107

Chapter Fourteen
"I Want Some Methylamine!"

To make MDMA, one absolutely has to have methyl-

amine. Similarly, to make meth from phenylacetone, methyl-
amine is a required chemical. As a result, methylamine has
been a hot item with the narco swine since well back in the
late seventies. Methylamine now sits on the notorious List I,
and is a definite "do not purchase or do business with people
who sell it" item.
Through the various editions of Secrets of Methamphet-
amine Manufacture, a procedure taken from Organic Synthe-
ses for making your own methylamine has been given. This
procedure is quite practical, and gives reasonably good re-
sults. Now other processes will be given that offer advan-
tages of their own, along with their own process specific dis-
advantages. Pick and choose for the method best suited for
your situation.

Method One - The Pipe Bomb

This method is taken from US Patent 2,085,785. It offers

good yields of methylamine in a shorter reaction time than
that required using the procedure from Organic Syntheses.
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Also, the chemical glassware "kit" isn't needed to make

methylamine by this method. A heavy steel pipe reaction
vessel and a heater will make the methylamine. Then a good
aspirator for vacuum, and a vacuum evaporation chamber are
required to recover the crystals of methylamine hydrochlo-
ride.
The method has the further advantage of replacing the
formaldehyde used in the Organic Syntheses process with
methanol. Both of these chemicals are easily available from
suppliers of industrial chemicals in both 5 gallon pails and
55 gallon drums, not to mention in smaller amounts from
hobbyist mail-order chemical outlets. The difference comes
in that methanol (wood alcohol) is even more widely used
than formaldehyde. You may even be able to fmd it on the
local hardware store shelf, or get them to order you a pail of
it. You just can't pass up hardware store chemicals when
they are available. HEET is fairly pure methanol.
Both of these methods use ammonium chloride as the
other ingredient to make methylamine. This material is easily
available from industrial chemical suppliers in 50 pound
bags, and in smaller amounts from "hobbyist" chemical
outlets. A common use for larger quantities is to slow the
melting of snow on ski slopes or sled runs. Craft a company
name accordingly.
To produce methylamine hydrochloride by this method,
one starts with a section of heavy steel pipe of about 2 quart
volume. It must be threaded on both ends, and matching
screw-on end caps obtained. Steel pipe is generally heavily
galvanized with zinc. This must be removed by immersing
the pipe and end caps in 5% HCI solution until the initially
vigorous fizzing slows to a crawl. Then rinse the pipe thor-
oughly in clean water to remove residual acid.
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Now screw the cap on the bottom of the pipe, and tighten
it down with a pipe wrench. It's best to then weld this cap
into place.
Next put 400 ml of methyl alcohol (methanol) into the
pipe, along with 535 grams of ammonium chloride, 400 ml
of water, and 2.5 grams of ferric chloride. This common
chemical often comes as a 40% solution in water for indus-
trial waste water treatment purposes. About 5 ml of this
solution would be plenty for the purpose. Mix the ingredients
thoroughly, then screw on the top cap. Tighten it down with
a pipe wrench as well.
The reaction mixture must be heated at 290 0 C to 300 0 C
for about two hours. To reach this temperature, the same
procedure as given in Chapter Seven should be used. A pot
filled with solder should be heated until it melts at about
400 0 F (205 0 C). The pipe should then be put in the pot, and
the temperature of the pot raised to the desired temperature.
Maintain this temperature for a couple of hours. A pressure
of hundreds of pounds per square inch will develop inside
the pipe, so don't hover around it while it cooks.
When the cooking period is over, turn off the heat and
remove the pipe from the pot before the solder solidifies.
When it is cool, the cap can be removed, and the contents
poured into a large filtering flask. The main reaction product
is methylamine hydrochloride, along with some unreacted
ammonium chloride and methanol, and some dimethylamine
hydrochloride byproduct. The ferric chloride catalyst will
color the mixture reddish brown.
To get pure methylamine hydrochloride, the mixture
should be evaporated under a vacuum. Just stopper the top of
the large filtering flask, and apply aspirator vacuum and heat.
As the amount of crystals formed during the evaporation gets
copious, they should be filtered out and kept in a glass jar
with lid. The mother liquor should then be returned to the
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filtering flask for more evaporation. This process should be

continued until the volume of the mother liquor reaches
between 100-200 ml,
Next recrystallize the collected crude crystals of methyl-
amine hydrochloride. This process will remove ammonium
chloride, ferric chloride and dimethylamine hydrochloride
from them. Clean out the large filtering flask, then put all the
collected crystals in it. Add about a quart of 190 proof vodka
to the flask, and heat the contents using a boiling hot water
bath. Swirl the contents of the flask around as it gets hot.
When it is hot, allow the crystals to settle, then decant off the
vodka solution into another flask, and filter the vodka out of
the settled crystals. Combine the vodka from the decanting
and filtering, and cool it down in the freezer. Return the
crystals to the filtering flask.
When the vodka gets cold, crystals of pure methylamine
will form. Filter them out, and store them in a glass jar with a
lid. Return the vodka to the filtering flask to repeat the heat-
ing/decanting/filtering/cooling and crystal collecting process.
After a few runs through this process, all of the methylamine
hydrochloride will be leached out of the ammonium chloride
which remains undissolved in the vodka. The ferric chloride
will remain dissolved in the vodka, and should stay com-
pletely out of the product crystals. Ditto for the dimeth-
ylamine, which shouldn't form in enough quantity to reach
saturation in the vodka. The yield should be over a pound of
methylamine hydrochloride crystals.
It's a good idea to check for the presence of dimethyl-
amine hydrochloride in the product. This is done by taking a
sample of the product and placing it in a beaker. Add enough
chloroform that a slush is formed. Stir it around for a few
minutes, then filter. Allow the chloroform to evaporate away.
If crystals form from the chloroform, this is dimethylamine

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hydrochloride. If there is a significant amount, the entire

product should be rinsed with chloroform.
If a person has difficulty getting ferric chloride, it can be
easily made. Take iron or steel filings, and put them in a
beaker. Add 15% HC~ about 20 rnl per gram of iron, and
heat. The iron will dissolve as ferric chloride. One gram of
iron will make 3 grams of ferric chloride. If there is any trace
of blue or green color in the resultant solution, pass a stream
of air through the solution for about Yz hour to oxidize all the
iron to the +3 state. The correct solution color is yellow or
brownish yellow. Then boil off most all the acid, until the
steam no longer gives an acid reaction with pH paper. Some
additional water may have to be added to get all the acid out
during the boil down. Don't evaporate the liquid completely
away, as overheated ferric chloride will decompose.

Method Two - From Methyl Iodide

This method gives satisfying yields of very pure methyl-

amine hydrochloride, but it requires that one have methyl
iodide in addition to hexamethylenetetramine. The latter is
easily made from formaldehyde and ammonium hydroxide.
See Home Workshop Explosives in the RDX chapter for the
recipe. An additional problem with this recipe is that about a
week of reaction time is needed. That aside, it's very easily
done and is recommended if the required materials are at
hand.
To make methylamine hydrochloride by this method, dis-
solve 140 grams of hexamethylenetetramine in 1500 rnl of
190 proof vodka. It will be necessary to heat the vodka in a
hot water bath to get the hexamethylenetetramine to dissolve.
As a result, one should choose a reaction vessel which isn't