4-MMC problematic synthesis

Albert A

Don't buy from me
Resident
Joined
Aug 6, 2022
Messages
17
Reaction score
3
Points
3
I melted 100g Bk4 in
400 ml of NMP added 200 ml of 40% methylamine in water. After finishing I added water with baking soda (NaHCO3) 10% and 250 ml DCM.
I separated the organic part and washed 4 times with water.
I dried with MgSo4 and added 200 ml of cold acetone and started dropping 37% hcl acid.
The mixture turned a red color and after 12 hours in the refrigerator and washing 3 times with acetone approximately 25 g was obtained.

Dear friends, is it possible to do something with the remaining mixture?
save the situation?
 

Attachments

  • XdazP9seq6.jpg
    XdazP9seq6.jpg
    3.8 MB · Views: 154

Jesse_Pinkman_

Don't buy from me
Resident
Language
🇩🇪
Joined
Sep 23, 2022
Messages
158
Reaction score
75
Points
28
You should keep the acetone from washing and let it evaporate, there is always some product left inside which appears in the end of evaporation.
This is mixed with acetone and filter again.
 

Albert A

Don't buy from me
Resident
Joined
Aug 6, 2022
Messages
17
Reaction score
3
Points
3
What does that mean ''keep the acetone from washing" ?
 

Jesse_Pinkman_

Don't buy from me
Resident
Language
🇩🇪
Joined
Sep 23, 2022
Messages
158
Reaction score
75
Points
28
When you wash and filter your product, the hcl, you use acetone...or?
That acetone is dirty but has also some product left inside, so you collect it, but it into a bowl or whatever, just let this acetone evaporate at a place with fresh air and after 1 or 2 days, there will be a leftover. Put fresh icecold acetone on it, stir and you get "milk" again, with less than before, but why dispose? When you filter it, you get another few grams of hcl, which is dried, washed again until the acetone which flows through IT becomes clear. Then dry it and/or recrystallize it.
 
Top