this is a repost from a somewhat obscure thread in the newbie forum...
Post 322683 (missing)
(RoundBottom: "Chromic’s Methylamine.HCl", Newbee Forum) i don't think it was as visible as it would be in it's own thread, so here it is.
Written by RoundBottom (karma, money, sex belong to chromic)
Preface:
First, this is a first attempt at making any MeAm.HCl so what it is supposed to look and smell like is a complete unknown (but whooee bob stinky-twat smell is bang on). Second, RB really knows nothing about chemistry other than what RB has learned since attending the Hive. Also, RB has never written a lab report in his life, so if the format is really off, please make any needed edits.
Reagents:
· 179.7g Hexamine camping fuel tablets
· 500mL muriatic acid (31.45% HCl acid)
· 550mL MeOH
· 550mL Acetone
Apparatus:
· 1L distilling flask
· 500mL receiving flask
· standard distillation setup (with cooling)
· rubber hose
· 600mL beaker
· 1000mL beaker
· 1” egg stir bar
· stir plate
· mantle and controller
· filter flask
· Buchner funnel and stopper
· filter paper
· vacuum source
Notes:
· The white hexamine tablets were a very common, “green Canadian camping products” brand. The tablets were put into a baggie and crushed to fit into a 1L flask.
· Chromic’s write-up suggests mixing the muriatic acid with the Hexamine in the flask while it sits in an ice bath. No temperature increase was noted, so this may be unnecessary.
Procedure:
Set up distillation apparatus as usual. A rubber hose was run from the vacuum inlet on the vacuum adapter to a window to expel any fumes.
Mix the muriatic and hexamine until dissolved. Took about 15 minutes, but will vary depending on hexamine type.
A gentle reflux was maintained for about 7 hours at a temperature of about 80°C-85°C. The heat was turned up to start the distillation. Fluid started dripping into the receiving flask at about 102°C. At about 11.5 hours, grains of AmCl were observed mixing in the distillation flask.
After about 12.5 hours the temperature had raised to 107°C and the drip rate had slowed down to about 1 drop per 4-5 seconds. About 270mL of clear distillate was recovered. It shouldn’t be required and can be disposed of later.
The heat was turned off and the reaction contents were allowed to cool down while still stirring. The fluid in the distillation flask had a medium yellow colour to it, and was still clear. There was also a large amount of spongy looking solids in the distillation flask that did not harden after cooling down, but remained sort of mushy. Bubbles were still evolving even after the distillation flask was allowed to cool for about 45 minutes.
A note about smell: once the distillation flask was removed the smell was really evident. It will stay in the room and on the skin for a few days. If you can at all manage it, make a fume hood, do this outside, or at least with a fan blowing out the balcony door. Smelly-twat, rotten anchovies, smegma dick… take your pick, it’s pretty nasty. Don't expect to hold a dinner party there the next day. The rubber hose is only useful while the distillation apparatus is connected.
Once cool, the contents of the distillation flask were vacuum filtered with saran wrap to squeeze out as much liquid as possible. About 250mL of fluid was collected (murky and cloudy, dark urine coloured). The crystals were put into the 600mL beaker and covered with 150mL room temp MeOH, manually mixed with a spatula for about a minute, poured into the filter. The beaker was rinsed with about 50mL MeOH and poured into the filter funnel, and then vacuum filtered, again with saran wrap. The AmCl crystals were put on a Pyrex dish to dry and kept for future use. Once dry, the ammonium chloride weighed 104g.
The combined filtrate and MeOH washes were then put back in the distillation flask, and distillation was started again. A temp of 40°C was reached in 25 minutes and fluid started coming over (BP of MeOH == ~64.6°C)
The temp climbed up to 108°C over 5.5h. After about 300 minutes a white smoke started filling the distilling flask. This is what we are waiting for, the sublimation of the MeAm.HCl. "Distilling to dryness," means the flask doesn’t have any more water in it. It does not mean, "Boil the hell out of it till everything's crunchy"
Once the smoke appeared, the heat was turned off and the contents were left to cool and solidify for 30 minutes. Sorry, the appearance of the fluid at this point wasn't noted. Once cool, 350mL MeOH was poured into the distillation flask and a reflux condenser was put on the flask (actually, the condenser from the distillation phase can be used, as it is already set up and this isn't a heavy reflux). The heat was turned up again, and the solution was allowed to reflux for about 15 min.
While hot, the solution was decanted into a Pyrex dish (a 1000mL beaker is probably better). Either way, the container was covered with saran wrap and left on the counter for 2 hours until cool. It was then moved to the fridge and left overnight. In the morning the beaker was moved to the freezer for another 2 hours. The crystals were large crunchy flakes, and the remaining fluid had an amberish tint.
It was once again vacuum filtered with saran wrap. About 375mL of fluid was recovered. At this point the crystals were large, white, translucent, and crunchy.
The crystals were put into a 600mL beaker and washed with 200mL ice-cold acetone for 5 minutes, and again vacuum filtered with saran wrap. The crystals were then spread out in a Pyrex dish to dry. The crystals looked smaller, and had a slight grayish tint.
The remaining fluid was crashed with 300mL ice-cold acetone and about 1.5g of crystals fell out. It was decided that it wasn't worth boiling the liquid down to recover any more.
In total 98.2g of crystals were recovered.
i learned a thing or two from charlie dontcha know.