DCM or Toluene for 4-mmc

[1019er]

I'd like to know if its possible Toluene from Amazon wich is shipped in 25L Gallon is 1. safe to order ?
And 2. Is it possible to use this instead of DCM for the extraction?

If not is it possible to produce DCM on my own as a noob?

 

[loadingST]

Completely yes, in the time i was synthesizing it i was putting a little bit xylene into dcm to make its boiling point a little higher with successful yield 70-80% every time.

I woud suggest you to obtain some triethylamine for acid screwenger and use Toluene as only solvent, dont over heat it just ...

 

[1019er]

Thx
So my ingredients will be:

2B4M - 100 g
DCM - 300 ml (Toluene)
Methylamine 40% aq solution - 200 ml
Hydrochloric acid - 50 ml
Dry acetone - 200 ml

Am I'm getting this right?

So I will have to buy the 2b4m and methylamine here.
The other stuff I can get legally.

Looking forward to start synthesis!

 

[w2x3f5]

You are right, triethylamine increases the yield well, it is important to take not in full quantity, it is best to take methylamine 4 mol per mole 2b4m, toluene and similar substances are optimal solvents at a temperature of 60-65 degrees, nucleophilic substitution takes place in 2.5 hours. Dichloromethane is not the best solvent; it produces more by-products and impurities. It is also important to have the lowest possible concentration of 2b4m and the finished aminoketone in solvents, this will reduce the likelihood of side reactions, and the nucleophile should be kept at its maximum concentration in the solution.

 

[Wendy]

I guess butyl amine could work as long chain primary amines are less reactive, than in this case MeNH2 as a nucleophile, no? or one would end up with mixture with N-methyl and N-buthyl alkyl grups in final product?

triethylamine is perfect l see, due to steric hindrance but not available to me.

 

[w2x3f5]

butylamine is definitely a bad idea.

 

[TheVacuumGuy]

2.5 hour in 60c toluene ? And at which point is NMP added (as shown in complete video tutorial in benzene)?

 

[G.Patton]

Sodium bisulfite also a good option for HBr removal. An excess of methylamine also react with the acid.

 

[Wendy]

@G.Patton
Patron

What do you think about the suggestions writen above?

 

[G.Patton]

Toluene is already was mentioned in a topic dedicated 4-mmc synthesis. It also can be used.

 

[Osmosis Vanderwaal]

Can we get an ordered list of the preferred solvents? I have ethyl acetate but I'm not a big fan of it. I couldn't find DCM through legal channels, which I found odd because I can find a lit more sinister stuff legally. I could order toluene but I would just like to know my options.
How does triethylamine increase the yield? I noted it is an acid scavenger. What acid are we scavenging?

 

[G.Patton]

HBr after nucleophilic substitution reaction with methylamine. Read my comment above.

 

[WillD]

A little sodium or potassium hydroxide can replace triethylamine if necessary.

 

[Osmosis Vanderwaal]

So by scavenging you mean are just neutralizing the acid? I don't think this is in the synth using ethyl acetate that you posted. After the methylamine and reflux I'm going to add drop wise a (6 mol? 3 mol) NaOH solution To ph what?

 

[Dr. MMX]

honestly, toulene has only one pro - its good solvent for 1st synthesis, you can learn faster i believe. Then when you have some knowledge about the process you can jump on other solvents and see how easy it is

if its your 1st time I thinkk its really good idea. I started this way( wasnt councious thats very hard and very bad) but learned a lot very fast way