PMK Oil Synthesys From PMK (CAS 28578-16-7 Wax Form) Large Scale

[btcboss2022]

Hello,

Sorry I was very busy these days, all the methods that I posted have been done and tested by myself as I say in the same post, it's more many of them tested and only the best one posted.
Thanks.

 

[Handsomerx]

Why is there no reference to color of the oil and aqueous phases?

 

[btcboss2022]

Im not used to reference them but what do you need to know exactly?

 

[Handsomerx]

Like what is the color of the oil which separates to the bottom? My starting pmk is kind of a light brown color so I assume the oil which renders out should look similar to that.
What is the color of the aqueous layer upon separation? Mine is a sort of pale yellow green.

I thought it was standard operating procedure to mention the color of your product.
Anyway thank you! It’d be very helpful to hear back.

Side note…when you say “evaporate dcm” do you mean actually to let it sit with low heat to evaporate? Or are you talking about stripping it under vacuum.

thanks

 

[Selassi]

1kg P
1kg water
150gr NaOH

Mix and melt at 85/90 for 1hr

450gr Phos and again 1,5hr at 85/90

After should be immediate separation from the layers

 

[Sjeik]

Stirring needed doing the conversion ? Phos 85% ?

 

[hjames]

Can HCl conc. 18% be used?
And can sulphuric acid be used instead of HCl?

 

[G.Patton]

yes, you have to increase its volume proportionately

 

[hjames]

And what about sulphuric acid?
is there any difference in effectiveness between h2so4 and hcl?

 

[G.Patton]

Yes, you can use sulfuric acid as well.

 

[Woody1835]

Absolute lifesaver. Great work bro.

 

[Big_Dexter]

what equipment do i need to do this process?
and if i don't have a reactor, can i replace it with another equipment.

 

[Big_Dexter]

what equipment do i need to do this procedure?

 

[UWe9o12jkied91d]

Condenser, suitable vessel, aquarium pump, beakers, bucket/s, heatable container for bath either sand or water, funnnels
@Big_Dexter

 

[Nicoino]

Hi, if you start with the sodium salt, should the basification process with NaOH be skipped or is it needed?

 

[rothschild33]

Did the procedure exactly as stated. Used 63.75 grams of PMK wax. Yielded 73 ml weighing 84.8 grams.

Stopped short of distillation which explains the remaining impurity, after separating DCM, liquid was heated to 50C under vacuum to remove DCM.

I'm curious, what's the remaining impurity mixed with mdp2p if the DCM has evaporated? Rotovap will arrive in the month and curious if this liquid can be good enough for further synthesis.

 

[Handsomerx]

Looks good. Would you be so kind as to post your weights and procedure? Considering you scaled down to about 1/50th of the original write up I’d like to see what you did.

 

[Sue]

Am tired of seeing micro brew methods this is more like it... LOL
Thanks for the post I have been curious about the glycidates and have found a few great posts here on them.
Awesome post...

 

[K-Cyanide]

@rothschild33 Your P2P looks still cloudy a hint of containing water. In general this synthesis is quite "dirty" in terms of side reactions. Thats why a vacuum distillation is imho preferable, unless you do large batches. (> 10kg). The loss in yield is significant in anyway you do the distillation. As an example, a 500g PMK batch yielded 382g "dirty" MDP2P. After vacuum distillation the amount was 303g, over 20% less, though the product has certainly a high purity with a nice pale golden colour

 

[nedkellygang]

Hi would would be mol ratios and mol amounts for this reaction or what would be the amounts for this on 100g pmk glycidate scales

 

[Loki12]

@nedkellygang
Check out the Laboratory FAQ section of the forum, you can find out how to calculate your reactions in the thread I link below;

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/moles-grams-litres-and-chemical-calculations.5295/

 

[nedkellygang]

Appreciate that !

 

[lemon]

I've been trying this for a while and I came to the conclusion that I was most likely scammed.
When I add NaOH whole solution get dark and it just stays like that, after heating nothing happens, just after adding too much of acid then glycidate reappears again. After heating I get dark red oil which quickly became solid when cold. Even when heating glycidate just in water i get same dark red oil.
I already wasted 200g of this and even tried reduction with it and nothing...
I even don't know if this is PMK glycidate or chinese scammed me.
About solubility: it's insoluble in water and highly soluble in IPA

 

[Jordan Belfort]

Brother, you can redo the failed reaction.

Take 1L hot water, use 500 gram caustic, on the hot lye one kg of the glydicate and I don't know pour slowly 1.5L hydrochloric acid it will 100 percent come. Then oil goes to the bottem once successfully turned you don't need to reflux

 

[Jordan Belfort]

Whats the cas number of the glydicate, if its the low hield p then this method doesnt work you will burn the oil