need help with bmk/pmk gly

[krillin]

Hey all,
My friend is having trouble doing the whole Al/Hg synth with bmk and pmk gly. Are the steps correct as follows:
Hydrolisis; keeping organic layer as is; reductive amination; solvent distillation; extraction and crystallisation?

 

[WillD]

Approximately so. What's the problem? (edited: answered in PM)

 

[krillin]

After a 3h reflux @ about 85, one phase of very dark near-purple solution @ pH 1 stays. No mdp2p oil in sight, he thinks.

 

[Gofast]

There is a difference between PMK and BMK glycidate. To get mdp2p you need P glycidate. Are you (sure you're) using PMK?
Also there are different types of P on the market right now, so it would be important to know which one you have.

 

[krillin]

PMK glycidate that is like a wax at room temp. At around 30C it melts to oil.

 

[Gofast]

Unfortunately I don’t know this form. I’ve only had it as a powder. Why don’t yoy ask the seller to provide you with the conversion recipe?

 

[WillD]

Maybe you have full ether (no sodium salt) and need +one-step reaction with alkali solution, before acid

 

[chinacat]

William is spot on

 

[chinacat]

water, alkali, and hcl.

 

[krillin]

Thanks. BMK powder seems to crystallize back to wax after 1h stirring in alkali setting then acid for my friend.

 

[chinacat]

pretty sure with powder you do hcl+water.l

 

[krillin]

Makes sense, thanks

 

[chinacat]

did u ever have any success with this? I never got anything during gassing stage.

 

[krillin]

Maybe your organic solvent isn't anhydrous while bubbling? There are a lot of reasons possible, you can try crashing out the salt, once your solution is acidic, with acetone. If it comes out then you know it's the crystallization step that needs work

 

[krillin]

Optimally you want your mgso4 in powder, just preblend it once anhydrous. you can see that it did its job when you swirl and it moves freely without clumping together, and when you let it settle the solution is clear. Those 2 indicators together are usually pretty solid for my friend. The acetone crashing out method is just to see if your previous steps were successful as you'll see some mdma hcl crashing out after adding large amount of acetone and putting it in the cooler. If everything worked well you should't have to check pH first you will see your mdma hcl crystallizing first. The pH is mostly to be sure that you've crystallized all the freebase.

You can add Hcl aq but then yes you will have to evap the hcl, if you use a gasser you will skip the evap step. Just add hcl aq to salt, I believe there is a detailed and clear procedure for this on this forum.