Sciencemadness Discussion Board

A good way to methylamine hcl by nitromethane reduction with fe/hcl?

Chemist1357 - 18-11-2022 at 01:56

Does anyone have a good workup or had success on making methylamine hcl from pure nitromethane? I'm done with the mess of ammonium chloride and formaldehyde.

I know there has been some talk about it but can someone list a synthesis with theoretical amounts?

John Black Super Chemist on youtube had this:

Nitromethane: 53.68ml
32% HCL: 150ml
Iron: 170

But A german named Krause had this:
1 mol of nitromethane or nitroethane
4.4 mol iron (pulverized cast iron filings, just use powder or more time)
about 1,5 mol Hcl
280 ml water

That is an enormous amount of iron! Here's a reference: https://www.thevespiary.org/rhodium/Rhodium/Vespiary/talk/in...

Thanks!

iLLCiD - 22-11-2022 at 10:17

Always thouight it might be able to be accomplished with NaBH4/CuCl2 but have never tried.

Texium - 22-11-2022 at 12:22

Enormous amounts of iron are typically used because these reactions are not the most efficient and iron is extremely cheap, so using a huge excess is not a problem and may be necessary to get the reaction to go to completion.

Mateo_swe - 24-11-2022 at 06:29

If you dont do this for the learning experience you could always just buy it.
If in Europe S3-Chemicals have both methylamine, ethylamine as well as many other intresting chemicals in their webshop.
https://shop.es-drei.de/

Or you can get it from one of the guys in "Reagents and Apparatus Aquisition " section of this forum.
I can recomend chemship1978.

kmno4 - 24-11-2022 at 18:02

Quote:

1 mol of nitromethane or nitroethane
4.4 mol iron (pulverized cast iron filings, just use powder or more time)
about 1,5 mol Hcl
280 ml water


It works without problems. For this amout of MeNO2 I would make 1 dm3 of total volume (see solubility of MeNO2 in water), with 1,2-1,3 mole of HCl. Do not use iron powder - very likely you will get hard mass of Fe+Fe3O4. Use small pieces (1cm x 1 cm) of sheet metal, nails, wire...., zinc coating makes no difference for the reaction. Frequent shaking of the mixture is important. When odour of MeNO2 dissapears and the mixture generates no more heat, reduction is finished. Yield is better than 90% .

Chemist1357 - 24-11-2022 at 21:45

Quote: Originally posted by kmno4  
Quote:

1 mol of nitromethane or nitroethane
4.4 mol iron (pulverized cast iron filings, just use powder or more time)
about 1,5 mol Hcl
280 ml water


It works without problems. For this amout of MeNO2 I would make 1 dm3 of total volume (see solubility of MeNO2 in water), with 1,2-1,3 mole of HCl. Do not use iron powder - very likely you will get hard mass of Fe+Fe3O4. Use small pieces (1cm x 1 cm) of sheet metal, nails, wire...., zinc coating makes no difference for the reaction. Frequent shaking of the mixture is important. When odour of MeNO2 dissapears and the mixture generates no more heat, reduction is finished. Yield is better than 90% .


Have you tried this reaction? the reaction you posted or the one I posted.