Need help in 4 MMC SYNTHESIS

[Lex369]

In my first synthesis of 4 MMC i followed genral procedure of 100 gram of bromoketone 200 ml 40 % methylamine and 300ml dcm 2hour 40 c temp posted on thread
And crystallization in 50/50 ipa water solution
I got 14 gram yield in first precipitation then remaining mother liquor and washing with acetone i put it again in freezer then get 6 gram precipitate
After doing crystallization crystals power are very low only half hour duration
How to increase power of the product and how to increase yield or any other procedure of of high yield high power synthesis of 4MMC i have 800 gram of 2 bromo 4 methyl propiophenone so i can do plenty of research on new procedures .

 

[$!$]

Is much more Simple and raster to do IT with no labo equipment

 

[superpamrz]

Like in PET bottles? Or glass jar just closed with some tape?

 

[$!$]

Simple

 

[chenkennywin]

I also encountered poor performance in terms of production capacity. After doing it several times, I roughly understood that if the purity and quality of monomethylamine aqueous solution (40%) is not good, it will directly affect production capacity, and too short a mixing reaction time is also a factor. one. I hope there are seniors who are good in the 4mmc field who can give me some pointers and provide them with powerful technology.

 

[Kiteretsu_D]

Whats up brother, can we talk in chat?

 

[Lex369]

Mephedrone onset of action and duration is very low by default or purity and production techniques matters

 

[Dr. MMX]

I believe you exceeded temp on some process it affects its power and yield, or maybe too high temp while acifification was in progress. we need more details what you exactly did to help, we cant do that unless you tell us
@

saifali899​

 

[Lex369]

I performed 100 gram 2b4mp 200 ml 40 %methylamine 300 ml dcm procedure 2 hours 40 Celsius and 30 mins mixing methylamine after getting layer i washed 3 times then 35 % hcl acidification but i didn't add acetone in acidification then i put in freezer in get precipitate after 12 hours i got 14 gram product and that product filtration with washed acetone that i agin put it in fridge i got 6 grams of precepitation

 

[$!$]

On dcm i was get 88g u made some mistake

 

[DavidNichols]

93% yield is impossible under your conditions.

 

[$!$]

Is small steps where u can made mistake

 

[rick001]

these are mephedrone crystals ?

 

[$!$]

Pure product

 

[DavidNichols]

Crystal system you have on the first photo diverge with one racemic mephedrone HCL should form. What are results of melting point measuring and TLC?