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]

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.

btcboss2022Why is there no reference to color of the oil and aqueous phases?

 

[btcboss2022]

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

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

 

[Handsomerx]

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

btcboss2022Like 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]

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

SelassiStirring needed doing the conversion ? Phos 85% ?

 

[hjames]

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

 

[G.Patton]

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

hjames

Can HCl conc. 18% be used?

yes, you have to increase its volume proportionately

 

[hjames]

yes, you have to increase its volume proportionately

G.PattonAnd what about sulphuric acid?
is there any difference in effectiveness between h2so4 and hcl?

 

[G.Patton]

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

hjamesYes, 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]

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.

View attachment 12756

rothschild33Looks 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]

@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/

Loki12Appreciate that !