MDP2P From PMK Glycidate

[JoeShmo]

I have been out of the game for years.. i ran a operation for a while that i did 250g batches using Al/Hg method. I have made mdp2p all the way from shaving sass root bark until i discovered PMK glycidate. BIG game changer lol. Anyways ive found myseld getting back into the action again and have sourced a PMK supplier. I ordered 2kg of oil from them ( they sat in freezer for a yr while building out the lab) I distillled them and they were very yellow. anyways went ahead did my al/hg reaction and low and behold didnt get a single thing not a gram.. and take in mind that i ran this reaction for years i know it like the back of my hand.. so i said fuck it the shits gone bad. Tossed it out and bought some pmk glycidate. Which brings me to my question. when i used to distill my pmk oil i always got water white beautful mdp2p that never froze in the deep freezer.. became very thick like syrup but never froze. I just finished distilling about 1.2l last night and stuck it in the freezer and the whole thing has frozen into beautiful super white clear crystal. IS THIS NORMAL? i dont remember my mdp2p freezing.

also just getting on here this is a beautiful site, i miss the hive. looking for a reaction for using methylamine hcl and not have to gas it, and a nabh4 route so i can scale to at minimal doing 1 kg at a time. i dont wanna mess with the small 250 reactions anymore and i hate cutting that much foil. anyone got a a good thread? i saw someone posted labtops old nabh4 route but he gasses.. i wanna just dissolve it in methanol.. is there a diff method for that?

Thanks Family Looking Forward To This New Site And Picking Brains Of People More Experienced Than Me.

 

[rothschild33]

You can slowly basify the methylamine hcl with sodium hydroxide to get methylamine freebase.

How was your MDP2P distillation setup? I'm currently working on optimizing my steam distillation, planning on adding potassium carbonate to increase yield from 225 ml distilled water with only 3 ml MDP2P in it

 

[JoeShmo]

Hey, thanks for the response. I use a very basic setup for distilling.. but i have a vacuum that pulls like crazy. its a really nice one. I use a magnetic stirrer, with my 3l fabric glas-col heating mantel on it.. three way adaptor, temp rig ontop.. regular 300mm liebig... vacuum takeoff and my receiving flask.. very plain and simple.. used to use the overhead vigreux column but when doing pmk oil i found it time consuming and not necessary.. i always get water white clear high grade oil.

steam distill.. why? so you dont gotta get a vacuum? i pull at about 130c at 1 torr.. my old vacuum had me pulling at 160 at about 10torr

so i really need this question addressed though if you have experience with it or if anyone else wants to chime in.. is mdp2p supposed to freeze?? Ive never had it happen before and this new suppliers stuff freezes.. is this not mdp2p? other than dropping a batch how else can i tell without serious lab equipment?

 

[rothschild33]

You're right, I should try vacuum distillation. I have a rotary vane vacuum pump 1 hp but overheats in 20 mins, will see if I can work around that find solutions.

I usually test my ketones with sodium bisulfite and see if it makes an adduct.

 

[JoeShmo]

Hey, Thanks Rothschild33. I had not heard of that test before, but doing a little bit of easy reading proves that yes that would at least show that a ketone or aldehyde is present. thats a starting spot at least.. i guess just running another batch would be the only sure fire way to prove it. I hit up the supplier and they said yes it freezes.. ive just never seen it happen before.

anyways i really appreciate your response, i kinda figured some other people might chime in based on all the views.
this would have to be something very common to people who work with mdp2p since your supposed to store it in the freezer.

 

[Nicoino]

Are you even serious?
Seriously man I'm really surprised you even had success in any synth.
PMK methyl/ethyl glycidate IS NOT PMK. Otherwise there wouldn't be the two words methyl/ethyl glycidate after it, don't you think?
It CANNOT be used for synthesis for the simple reason it is not a KETONE.
you have to hydrolize and decarboxylate it yield PMK, which later can be used for synth.

 

[JoeShmo]

so your telling me that after i drop the powder back to oil and distill it it is not ketone? i mean this throws my mind so far off.. i produced kilos of mdma that had been lab tested for purity by energy control in spain.. i did this doing this exact method. i would reflux the powder in acidic water for an hour and the oil drops out.. collect the oil.. neutralize it by washing . distill it and used it.. did it for years

 

[Nicoino]

You didn't mention any hydrolysis in your post, which is very unclear.
Also if you start with PMK et-gly you need a basic hydrolysis first to get the carboxylic acid from the ester and then the HCl process to convert the epoxide to ketone liberating CO2.
If your start material is real and you do the correct process you will get high quality PMK which works wonderfully for synth.

 

[JoeShmo]

Yeah after i typed a response to you including the hydrolysis i sat back and was like i bet thats what your meaning.. yes anyone working with pmk glycidates should be safe to assume they just already know how to convert it back into pmk.. sorry for the confusion there.

 

[JoeShmo]

but whats up anyone else know about the mdp2p freezing into crystal?

 

[metux]

I can't find why did from PMK Oil,?

 

[Rabidreject]

My understanding, and I was just about to ask about this, is that you have to react it with an acid (I read HCL but can’t remember what strength - think it was 35%) and then proceed with the PMK.

I need to do some reading on the area but my understanding was that after that you just need to do a reduction.
Am I even correct in this?

I am awaiting an aspirator and I have pretty good water pressure so we’ll c what it can pull.

Anyway - back to the reading about it lol

 

[Rabidreject]

Oooh okay so you to perform an acid/base reaction by the look of things…my bad

 

[Rabidreject]

My other question still stands though, can you get away with using NaBH4 instead of something like LiAlH4

 

[Rabidreject]

Oh also, I mean for the final step once you have your MDP2P for the reductive amination….obviously haha I dunno why I felt I had to clarify that to a room full of chemists!

 

[Rabidreject]

Oh and as for freeze point can’t you simply lookup the freezing point of MDP-2-P? Or is it the glycidate you are talking about freezing?