hello so ur interestin in makin methylamine huh?
i got chu!
(credit out to EHRMANTRAUT for having the idea of making this guide)
so to start off there are quite a few ways to make methylamine so thats why my favorites will be ranked from top (best) to bottom (absolute dogshit).
nitromethane reduction route:
what u need:
- nitromethane 50g
-zinc 137.5g
- 350.6ml 30% HCl
- solvent for the methylamine e.g. methanol , water (or if u desire methylamine Hydrocloride HCl can also be used)
- 228.6g NaOH disolved in a minimal amount of water
first the 50g nitromethane and the 137.5g zinc were addet to a 2 neck round bottom flask equipped with a addition funnel and a reflux condensor
then the 350.6ml 30% HCl was addet into the addition funnel and subsequently slowly dripped in.
meanwhile the solvent was put into a fridge or icebath to cool it down.
after all the HCl was addet the opening of the reflux condensor was equipped with a gas adapter with a tube atached leading into a beaker filled with the solvent ( for a slightly higher yield the beaker was put into a ice bath)
the NaOH was addet to the addition funnel and addet very slowly to the reaktion mix.
after the addition of the NaOH solution was complete the reaktion mix was brought to a reflux for 5 min.
et voilà u now have a methylamine solution in the beaker.
( if u want it azeotropic just destill it)
also u can reduce the nitromethane with Hg/Al amalgam if u want to for some reason.
acetamide hoffman rearangement route:
what u need:
- ammonia
- acetic acid aka vinegar
- 20g calcium hypocloride disolved in a minimal amount of water
- 20g NaOH also disolved in a minimal amount of water
- solvent for the methylamine e.g. methanol , water (or if u desire methylamine Hydrocloride HCl can also be used)
firstly a randome amount of vinegar was addet to a beaker and ammonia was addet till the solution turns basic .
then all the water and ecess ammonia was boiled off and the rest of the solution was addet to a round bottom flask equiped with a reflux condensor and subsequently refluxed for 3h.
after thats done the reflux condensor was replaced with a shortpath destilation adapter ( do not put water in the condensor otherwise it will clog) witch was equipped with a thermometer.
the solution was now destilled and any destilate that comes over at under 150c was discardet.
(if the destilate that comes over at over 150c doesnt cristalise in the recieving flask just scrape the flask bottom with a stirr rod and it should cristalise)
with the acetamide now made the methylamine fun can now begin.
(u can also just start off with acetamide and skip all of that and just start off with bought acetamide)
10g of acetamide was disolved in a minimal amount of water.
meanwhile the solvent was put into a fridge or icebath to cool it down.
the acetamide solution was then transfered to a 2 neck round bottom flask placed in a salt ice bath witch was equiped with a addition funnel and a stopper
the calcium hypocloride solution was now put into the addition funnel and addet extremly slowly so that the temperature of the reaktion mix doesnt exceed 10c.
after thats done the whole set up was then put out of the ice bath
and then NaOH solution was quickly poured in.
(the stopper was replaced with a reflux condensor witch was equipped with a gas adapter conected to a tube leading into a beaker with ur cold solvent of choice in it (beaker can be placed into a ice bath for a higher yield) and the addition funnel was replaced with a stopper)
and finaly the reaktion mix was refluxed for 3h
et voilà u now have a methylamine solution in the beaker.
( if u want it azeotropic just destill it)
Hexamine decomposition method:
what u need:
- 70g hexamine disolved in 120ml water
-244.3ml 30% HCl
-NaCO3 disolved in a minnimal amount of water
- solvent for the methylamine e.g. methanol , water
to start off the hexamine solution was put in a 2 neck round bottom flask and the HCl was slowly addet.
after all the HCl was addet the flask was equipped with a thermometer and a destilation set up.
now its just 1/1 the same procedure as with the ammonium cloride formaldehyde route.
ammonium cloride and formaldehyde route:
what u need:
-100g ammonium cloride
- 208ml 37% formaldehyde (methanol stabilised )
-NaCO3 disolved in a minnimal amount of water
- solvent for the methylamine e.g. methanol , water
to start off the ammonium cloride and formaldehyde were addet to a 2 neck round bottom flask equipped with a thermometer adapter and a destilation set up and the heat was increased till the thermometer reads around 100c
after the destilation slowed to a crawl a vacuum was aplied till ammonium cloride crashes out.
the reaktion mix was then alowed to cool down in a freezer and subsequently filtered (the shit left in the filter is ammonium cloride and can be re used for more runs)
this was then repeated 2 times.
the seccond time was still majorly ammonium cloride left in the filter and the third time it should be mostly pure methylamine HCl.
this methylamine HCl was then recristalised.
at last this was then just freebased by adding the NaCO3 solution to it and bubbeling the methylamine trough the solvent of choice.
found a vid on this method:
fin.
i got chu!
(credit out to EHRMANTRAUT for having the idea of making this guide)
so to start off there are quite a few ways to make methylamine so thats why my favorites will be ranked from top (best) to bottom (absolute dogshit).
nitromethane reduction route:
what u need:
- nitromethane 50g
-zinc 137.5g
- 350.6ml 30% HCl
- solvent for the methylamine e.g. methanol , water (or if u desire methylamine Hydrocloride HCl can also be used)
- 228.6g NaOH disolved in a minimal amount of water
first the 50g nitromethane and the 137.5g zinc were addet to a 2 neck round bottom flask equipped with a addition funnel and a reflux condensor
then the 350.6ml 30% HCl was addet into the addition funnel and subsequently slowly dripped in.
meanwhile the solvent was put into a fridge or icebath to cool it down.
after all the HCl was addet the opening of the reflux condensor was equipped with a gas adapter with a tube atached leading into a beaker filled with the solvent ( for a slightly higher yield the beaker was put into a ice bath)
the NaOH was addet to the addition funnel and addet very slowly to the reaktion mix.
after the addition of the NaOH solution was complete the reaktion mix was brought to a reflux for 5 min.
et voilà u now have a methylamine solution in the beaker.
( if u want it azeotropic just destill it)
also u can reduce the nitromethane with Hg/Al amalgam if u want to for some reason.
acetamide hoffman rearangement route:
what u need:
- ammonia
- acetic acid aka vinegar
- 20g calcium hypocloride disolved in a minimal amount of water
- 20g NaOH also disolved in a minimal amount of water
- solvent for the methylamine e.g. methanol , water (or if u desire methylamine Hydrocloride HCl can also be used)
firstly a randome amount of vinegar was addet to a beaker and ammonia was addet till the solution turns basic .
then all the water and ecess ammonia was boiled off and the rest of the solution was addet to a round bottom flask equiped with a reflux condensor and subsequently refluxed for 3h.
after thats done the reflux condensor was replaced with a shortpath destilation adapter ( do not put water in the condensor otherwise it will clog) witch was equipped with a thermometer.
the solution was now destilled and any destilate that comes over at under 150c was discardet.
(if the destilate that comes over at over 150c doesnt cristalise in the recieving flask just scrape the flask bottom with a stirr rod and it should cristalise)
with the acetamide now made the methylamine fun can now begin.
(u can also just start off with acetamide and skip all of that and just start off with bought acetamide)
10g of acetamide was disolved in a minimal amount of water.
meanwhile the solvent was put into a fridge or icebath to cool it down.
the acetamide solution was then transfered to a 2 neck round bottom flask placed in a salt ice bath witch was equiped with a addition funnel and a stopper
the calcium hypocloride solution was now put into the addition funnel and addet extremly slowly so that the temperature of the reaktion mix doesnt exceed 10c.
after thats done the whole set up was then put out of the ice bath
and then NaOH solution was quickly poured in.
(the stopper was replaced with a reflux condensor witch was equipped with a gas adapter conected to a tube leading into a beaker with ur cold solvent of choice in it (beaker can be placed into a ice bath for a higher yield) and the addition funnel was replaced with a stopper)
and finaly the reaktion mix was refluxed for 3h
et voilà u now have a methylamine solution in the beaker.
( if u want it azeotropic just destill it)
Hexamine decomposition method:
what u need:
- 70g hexamine disolved in 120ml water
-244.3ml 30% HCl
-NaCO3 disolved in a minnimal amount of water
- solvent for the methylamine e.g. methanol , water
to start off the hexamine solution was put in a 2 neck round bottom flask and the HCl was slowly addet.
after all the HCl was addet the flask was equipped with a thermometer and a destilation set up.
now its just 1/1 the same procedure as with the ammonium cloride formaldehyde route.
ammonium cloride and formaldehyde route:
what u need:
-100g ammonium cloride
- 208ml 37% formaldehyde (methanol stabilised )
-NaCO3 disolved in a minnimal amount of water
- solvent for the methylamine e.g. methanol , water
to start off the ammonium cloride and formaldehyde were addet to a 2 neck round bottom flask equipped with a thermometer adapter and a destilation set up and the heat was increased till the thermometer reads around 100c
after the destilation slowed to a crawl a vacuum was aplied till ammonium cloride crashes out.
the reaktion mix was then alowed to cool down in a freezer and subsequently filtered (the shit left in the filter is ammonium cloride and can be re used for more runs)
this was then repeated 2 times.
the seccond time was still majorly ammonium cloride left in the filter and the third time it should be mostly pure methylamine HCl.
this methylamine HCl was then recristalised.
at last this was then just freebased by adding the NaCO3 solution to it and bubbeling the methylamine trough the solvent of choice.
found a vid on this method:
fin.