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All 7 posts Subject: Methylamine clean-up Please login to post Down

aleph
(Stranger)
08-20-03 15:34
No 454708
      Methylamine clean-up

I dreamed of making methylamine from formaldehyde and ammonium chloride. Everything went according to text until the end - the crystals would supposedly form in the hot solution after volume reduction, and be somewhat brown. My crystals formed only after I turned off the heat plate and the solution started cooling, and they are very brown. Anyone know a simple way to clean up these crystals? Also, is methylamine supposed to smell like a dog in heat, or did I dream a screw-up?

raffike
(Hive Addict)
08-20-03 15:38
No 454709
      Chloroform will clear that shit up.Or if not...

Chloroform will clear that shit up.Or if not then try acetone.Smell is right.. laugh

For those about to synth,we salute you

biffman
(Stranger)
08-23-03 21:30
No 455248
      Methylamine cleanup

First you should rinse with chloroform to remove any dimethylamine but then you definitely should be purifying the methylamine by re-crystalization. If you can get it, and if you can put up with the lovely smell, n-butyl alcohol works better than ethanol.
Reflux your crystals in the alcohol and get as much into solution as possible then decant (or filter) and let cool. The methylamine will come out nicely. Filter off the crystals. Repeat as many times as necessary. I found that to get the final smelly n-butyl alcohol out of the methylamine rinse with isopropyl alcohol then acetone.

raffike
(Hive Addict)
08-24-03 07:19
No 455367
      wet ethanol doesn't work,it contains too much...

wet ethanol doesn't work,it contains too much water and methylamine is pretty soluble ethanol aswell,propyl/butyl alcohol should work just fine

For those about to synth,we salute you

technology
(Hive Bee)
08-24-03 08:41
No 455381
User Picture       In order to obtain a pure product, the crude...

In order to obtain a pure product, the crude methylamine hydrochloride is recrystallized from absolute alcohol. The crude salt is placed in a flask fitted with a reflux condenser protected at the top with a calcium chloride tube. Absolute alcohol is added and the mixture heated to boiling. After about one-half hour the undissolved material is allowed to settle and the clear solution is poured off. When the alcoholic solution is cooled, methylamine hydrochloride crystallizes out. It is filtered off, and the alcohol used for another extraction. The process is repeated until the alcohol dissolves no more of the product (about five extractions are necessary). In the flask. you still end up with ammonium chloride remains. And the result being recrystallized methylamine hydrochloride.

Since ammonium chloride is not absolutely insoluble in 100 per cent ethyl alcohol (100 g. dissolve 0.6 g. at 15°), the methylamine hydrochloride purified in the manner described contains appreciable traces of it. A purer product can be prepared by recrystallizing from n-butyl alcohol, in which the solubility of ammonium chloride even at the boiling temperature is negligibly small. Methylamine hydrochloride is somewhat less soluble in this solvent than in ethyl alcohol, but as a rule three extractions carried out at 90–100° with 4–6 parts of fresh butyl alcohol for each extraction result in a substantially complete separation. Since the last traces of the solvent are not readily removed by exposure to air, a solution of the recrystallized material in a small quantity of water should be distilled until free of alcohol, and allowed to crystallize

all the best, tongue tongue tongue

Without GLASSWARE where the fuck would we BEE?

aleph
(Stranger)
08-24-03 15:47
No 455403
      thanks, bees

Thanks for the info Bees

NeoSynthesis
(Hive Bee)
10-11-03 23:23
No 464080
      Correct me if i'm wrong Tech

Ok.. Not sure about the part with the CaCl tube, but if i understood you correctly, what you're sayin is that the MeAm xtals are boiled/refluxed in a flask of "Absolute Alcohol" (volume?) for about half-an-hour to an hour. Whatever settles to the bottom is basically crap. The solution is allowed to cool down to r/t, at which point the MeAm xtals come out of solution, are filtered out (not sure if you mean vac-filtered?) and then the remaining absolute alcohol is good to go for your next batch?

Also, you said that n-butyl alcohol (if can be obtained) is better for this then absolute alcohol (solubility of NH₄Cl, etc). Would the clean up be done the same way?

What did you mean by:

"but as a rule three extractions carried out at 90–100° with 4–6 parts of fresh butyl alcohol for each extraction result in a substantially complete separation"?

Last thing: Does either one of these clean up jobs remove foreign smell from the MeAm xtals that result from the synth? And.. do these clean ups REPLACE chloroform or acetone washing? (mind you.. if you wouldn't mind explaining how chloroform/acetone washes are carried out, I would be much obliged)

Thanks in advance - Peace out

Houston................?????????????

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	All 7 posts		Subject: Methylamine clean-up		Please login to post		Down


		aleph (Stranger) 08-20-03 15:34 No 454708				Methylamine clean-up
						I dreamed of making methylamine from formaldehyde and ammonium chloride. Everything went according to text until the end - the crystals would supposedly form in the hot solution after volume reduction, and be somewhat brown. My crystals formed only after I turned off the heat plate and the solution started cooling, and they are very brown. Anyone know a simple way to clean up these crystals? Also, is methylamine supposed to smell like a dog in heat, or did I dream a screw-up?



		raffike (Hive Addict) 08-20-03 15:38 No 454709				Chloroform will clear that shit up.Or if not...
						Chloroform will clear that shit up.Or if not then try acetone.Smell is right.. For those about to synth,we salute you



		biffman (Stranger) 08-23-03 21:30 No 455248				Methylamine cleanup
						First you should rinse with chloroform to remove any dimethylamine but then you definitely should be purifying the methylamine by re-crystalization. If you can get it, and if you can put up with the lovely smell, n-butyl alcohol works better than ethanol. Reflux your crystals in the alcohol and get as much into solution as possible then decant (or filter) and let cool. The methylamine will come out nicely. Filter off the crystals. Repeat as many times as necessary. I found that to get the final smelly n-butyl alcohol out of the methylamine rinse with isopropyl alcohol then acetone.



		raffike (Hive Addict) 08-24-03 07:19 No 455367				wet ethanol doesn't work,it contains too much...
						wet ethanol doesn't work,it contains too much water and methylamine is pretty soluble ethanol aswell,propyl/butyl alcohol should work just fine For those about to synth,we salute you



		technology (Hive Bee) 08-24-03 08:41 No 455381				In order to obtain a pure product, the crude...
						In order to obtain a pure product, the crude methylamine hydrochloride is recrystallized from absolute alcohol. The crude salt is placed in a flask fitted with a reflux condenser protected at the top with a calcium chloride tube. Absolute alcohol is added and the mixture heated to boiling. After about one-half hour the undissolved material is allowed to settle and the clear solution is poured off. When the alcoholic solution is cooled, methylamine hydrochloride crystallizes out. It is filtered off, and the alcohol used for another extraction. The process is repeated until the alcohol dissolves no more of the product (about five extractions are necessary). In the flask. you still end up with ammonium chloride remains. And the result being recrystallized methylamine hydrochloride. Since ammonium chloride is not absolutely insoluble in 100 per cent ethyl alcohol (100 g. dissolve 0.6 g. at 15°), the methylamine hydrochloride purified in the manner described contains appreciable traces of it. A purer product can be prepared by recrystallizing from n-butyl alcohol, in which the solubility of ammonium chloride even at the boiling temperature is negligibly small. Methylamine hydrochloride is somewhat less soluble in this solvent than in ethyl alcohol, but as a rule three extractions carried out at 90–100° with 4–6 parts of fresh butyl alcohol for each extraction result in a substantially complete separation. Since the last traces of the solvent are not readily removed by exposure to air, a solution of the recrystallized material in a small quantity of water should be distilled until free of alcohol, and allowed to crystallize all the best, Without GLASSWARE where the fuck would we BEE?



		aleph (Stranger) 08-24-03 15:47 No 455403				thanks, bees
						Thanks for the info Bees



		NeoSynthesis (Hive Bee) 10-11-03 23:23 No 464080				Correct me if i'm wrong Tech
						Ok.. Not sure about the part with the CaCl tube, but if i understood you correctly, what you're sayin is that the MeAm xtals are boiled/refluxed in a flask of "Absolute Alcohol" (volume?) for about half-an-hour to an hour. Whatever settles to the bottom is basically crap. The solution is allowed to cool down to r/t, at which point the MeAm xtals come out of solution, are filtered out (not sure if you mean vac-filtered?) and then the remaining absolute alcohol is good to go for your next batch? Also, you said that n-butyl alcohol (if can be obtained) is better for this then absolute alcohol (solubility of NH₄Cl, etc). Would the clean up be done the same way? What did you mean by: "but as a rule three extractions carried out at 90–100° with 4–6 parts of fresh butyl alcohol for each extraction result in a substantially complete separation"? Last thing: Does either one of these clean up jobs remove foreign smell from the MeAm xtals that result from the synth? And.. do these clean ups REPLACE chloroform or acetone washing? (mind you.. if you wouldn't mind explaining how chloroform/acetone washes are carried out, I would be much obliged) Thanks in advance - Peace out Houston................?????????????

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