Author Topic: Baals favorite Methylamine synth...  (Read 2265 times)

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brownhornet

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simpler than hcl/hexamine reflux???
« Reply #20 on: April 01, 2002, 06:10:00 PM »
chromic very interested in a simpler workup procedure than than hcl/hexamine vac reflux method.  not working, getting more ammonium chloride than methylamine.
conditions; 20mmhg vac,  80-85c reaction temp, 6-8hrs total. vac distilled to get mush then extract with methanol.
would like your help since baals method has got me stirred. rhodiums site under methylamine synth also mentions "at least 95% yeilds under vac reflux and distillation".
thnx bro

cheeseboy

  • Guest
Adding Formaldehyde
« Reply #21 on: April 01, 2002, 11:59:00 PM »
Jasium, so what you're saying is  that adding some formaldehyde to the mix will react with the the ammonium chloride to get even better yields and using the ammonium chloride instead of worrying about filtering it or having it as an impurity. And there is alot of ammonium chloride produced when using HCl to hydrolyse Hexamine. Brilliant jasium... jasium where are you? Oh ya, they took you away, always sorry to hear that.

May De Sorce Bee Wit Chu-Always

Flinger

  • Guest
Acedamide via pink eye??
« Reply #22 on: April 02, 2002, 01:23:00 AM »

Chromic

  • Guest
MeAmCl from hex/HCl
« Reply #23 on: April 02, 2002, 06:11:00 AM »
I don't believe that yields better than 50% (post-recrystallization) of pure scent-free flaky beautiful white snowflake-like crystals of methylamine hydrochloride can be acheived with this method or with the (para)formaldehyde/ammonium chloride method.

I'm very skeptical of anyone who claims otherwise. Notice how baalchemist never answered MaDMAx's question about the yields. 70g of hexamine (0.50mol) reacted with 200ml of 31.45% HCl (232g 31.45% HCl(aq), 72.96g HCl(g) ie 2.00mol of HCl) should in theory yield 101.1g of methylammonium chloride (ie 1.5mol of methylammonium chloride). So a 90% yield or whatever baal claims  would be like 90g. I have SEVERE reservations on the validity of that yield. I'd be lucky to get 50g from that run (ie 50% yield).

I really should post that write-up...

Chromic

  • Guest
oh yeah, that's because..
« Reply #24 on: April 02, 2002, 06:21:00 AM »
I should have mentioned that 3mol of MeAmCl should come from 1mol hexamine because each hexamine molecule becomes 6 formaldehyde and 4 ammonium chloride. 2 formaldehydes are needed for each molecule of methylamine (ie from 1 comes 6 comes 3... make sense?), and so there is excess ammonium chloride.

Chromic

  • Guest
just to get you started
« Reply #25 on: April 02, 2002, 06:33:00 AM »
Ok, brownhornet. Here's what I've done (short writeup):

70g hexamine, stir bar added to 250ml rb flask. 200ml of cold 31.45% HCl is added. The flask is setup for simple distillation. 100ml is *slowly* distilled off over about 12hrs (the slower the better). The flask is cooled, AmCl filtered off. The AmCl is washed with 50ml MeOH, the MeOH put back into the flask. The flask is then distilled until it starts to smoke (AmCl sublimating). Everything is allowed to cool. 125ml of MeOH is added. Refluxed for 5 min. The heat is turned off and it is cooled slowly and undisturbed to room temp. Then it's moved to the fridge. Then to the freezer. Then it's suction filtered with saran wrap to squeeze out all the liquid possible. Then the crystals are put in 60ml of acetone and filtered again. Then you can throw them into a vacuum dessicator if you've got it, or just spread them out on a surface at 70-90C. Normally yields about 45-50g. The yields aren't stellar but this is by far the easiest MeAm that gets you really good quality MeAmCl with not much work.

If anyone is unhappy about the quality of MeAmCl they are making, I invite you to try this. The purity is really good (esp compared to BS's method!).

Organikum

  • Guest
pressure conversion
« Reply #26 on: April 02, 2002, 09:26:00 AM »
It is possible that ya have thy same problem as I had some time ago.

UNIT CONVERSION

Baal says 22" vacuum, what means 22inch Hg and may be about 540mm Hg (or Torr).
If ya got down to 20mm Hg this seems to be a bit low.....
By my interpretation only a little vacuum was applied to get rid of thy fumes and to lower the boiling temperature just below thy magic 104°C.

Maybee
ORGY

"I hope I'm becoming more eccentric. More room, you know.
 More room in the brain."

RoundBottom

  • Guest
good enough for me...
« Reply #27 on: April 02, 2002, 09:51:00 AM »
chromic, if i could follow your writeup, then i'm sure most bees won't have a problem.  give both your and my writeups to rhodium, that should be enough info for all.

i learned a thing or two from charlie dontcha know.