Please advise on Akabori-Momotani reaction

[drN1mbis]

Good day to all.

Thank you for all the wonderful work done on this site.

Im planning to try to synthesise ephedrine with Benzaldehyde and methylalanine and reducing it with mercury almalgam.

Could anyone have a look at my plan and see if it will work.

*********************'


workout for the reaction between 30g benzaldehyde and 25g methylalanine:

*Reaction Conditions*

1. Solvent: DMSO (60-80 ml)
2. Reductant: Aluminum amalgam (3-4.5g Al, 0.3-0.45g Hg)
3. Temperature: 20-30°C
4. *Time*: 1 hours
5. *Stirring*: Magnetic stirrer

*Procedure*

1. *Prepare aluminum amalgam*: Mix 3-4.5g Al with 0.3-0.45g Hg.
2. Combine benzaldehyde and methylalanine and DMSO in different flask


3. aluminum amalgam gets prepared in a different flask adn the Benzaldehyde/methylalanine solution gets added in portions to Amalgam and temperature maintained at 20 celcius for 1 hour after last portion is added.

4. Filter out aluminum amalgam

5. add 25% Naoh solution until PH 13 and extract with Toluene x 3

Extract freebase from Toluene with 5% HCL solution and evaporate


Thanks for having a look. Some of the values were just made up so i can get the ball rolling

Any input with be appreciated dearly

 

[Acab1312]

Hello, this synthesis has been described here before by xoxo2.0, very well. Hir is the link

 

[Acab1312]

EPHEDRIN ZU HAUSE HERSTELLEN

MAKING EPHEDRINE BY SIMPLEST METHORD 20GM OF N-methyl-d,L-alanine 50GM OF benzaldehyde ADD IT IN A ROUND BOTTOM FLASK PUT IT IN A OIL BATH AT 150-160 DEGREE C. (NOTE: PUT THE FLASK IN OIL AT ABOUT 60 DEG. ) AND GRADUALLY INCREASE THE TEMPERATURE ABOUT IN THE TIME PERIOUD OF 30-40 MIN...

bbgate.com

I hope I could help

 

[drN1mbis]

Thanks homie, im gonna check it out right now

 

[drN1mbis]

Updated, the links was not helpful unfortunately.
It seems to be the method as described by Uncle fester in his books. Almost Verbatim

Ive heard different people mention reducing agents such as
NaBH4
LAH
Hg amalgam
To reduce the oxime that forms between Benzaldehyde and methylalanine

I want to find out if this it true

 

[drN1mbis]

I will be eternally grateful if an expert can shime in