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

[G.Patton]

This post is a good explanation, which was posted @btcboss2022 (thank you). I confirm, that it is a proven and working method.

 

[FredDurst]

Is there any alternative to DCM (Toluene maybe?) as its hard to get in my country?

 

[Precursor-supplier]

I can provide

 

[Jordan Belfort]

boiling of tolueen is problem.

 

[btcboss2022]

Hello,

Firstly I don't think you created that process, in fact I had this similar info long time ago from Chinese suppliers, anyway I made some changes as you can see.
Sodium bicarbonate is a softer washing method and in this case is safer to use it to avoid to damage the product.
About DCM obviously I mean to separate the bottom layer(DCM layer) and evaporate it sorry if my explanation is not clear.
To avoid water after separate layers you can dry it with anydrous sodium sulfate and filter it before evaporate the solvent( in fact I always do it in all my processes)
Thanks.

 

[FredDurst]

Is there any alternative to DCM (Toluene maybe?) as its hard to get in my country?

 

[btcboss2022]

Toluene will works too but I can't assure you the same yield basically because I didn't tried.

 

[FredDurst]

Ok thanks mate. Will give it a go

 

[J-man]

Hi everyone, sorry but is the starting material here, this PMK wax. Is this just Paraffin Wax, Piperonyl Methyl Ketone PMK? Or is this PMK wax something completely different? Thanks

 

[G.Patton]

Hello, there is CAS number in the heading

 

[J-man]

I guess another question would be is PMK glycidate oil the same thing as PMK Piperonyl Methyl Ketone? I have looked but still unsure as there are many answers saying Piperonyl Methyl Ketone is PMK? Thanks

 

[J-man]

Never mind lol, i just worked it out. so, this PMK you start with here- (PMK glycidate oil) is different to PMK Piperonyl Methyl Ketone.. you end up with PMK Piperonyl Methyl Ketone (MDP2P) (4676-39-5) after doing this PMK oil Synthesis!
Haha man.. Good times

 

[Handsomerx]

Sorry I’m new here. Can anyone answer two questions
Using CAS 25785 (pmk glycidate oil) then adding naOH, then adding sulfuric, oxalic, and citric acid over time and washing with H20, bi carb, brine, and vacuum distillation
1) what color should it be? Mine is a beautiful red color. Clear.
2) what does it smell like? Mine smells like…idk? Chemicals? But kinda sweet?
thanks in advanced
-handsome

 

[btcboss2022]

I don't know the process that you follow with that products but normally is a yellow-brown oil depends of PMK manufacturer too the best one I use the final oil is yellow.

 

[Handsomerx]

230 g pmk
Added to 300ml 16% naOH solution stired 2 hours
20%sulfuric acid 100 g citric 60 oxalic mixed cooled and added 30 mil at a time
Cooled to 30c added xylene until waiting until oil separated to tooe
H20 washes and bicarbonate washes if that helps

 

[btcboss2022]

Without heating and reflux?
And it works? Yield?
Interesting if it works but difficult to make the processes needed in good way without heating.

 

[Handsomerx]

Pardon 28578, same one you’ve written about.
yes heated in base phase and acid.
And heated during vacuum

 

[G.Patton]

It isn't PMK gycidate.

 

[Handsomerx]

Sorry that was a typo. Sometimes that dyslexia slides in.

 

[otw247]

Is it possible to substitute DCM for Toulene?

Sadly I'm in a country where DCM is heavily watched

 

[btcboss2022]

Yes possible but yield could change.

 

[bitcoinup2020]

Hello, I'm a beginner.

I would like to inquire in section 6.
6. Add 3,25kg of HCL 37% in small portions, once all added keep the mixture at 80 °C reflux during 1 hour stirring.

Can I use Hydrochloric Acid 35% instead of Hydrochloric Acid 37%?

 

[Zarder]

Yes you can. Just make sure the molar equivalences are the same

 

[otw247]

Just to confirm - can you make sure my maths are correct?

HCI 37% (0.37*1.18*(1000/36.46) = 11.97M

HCI 35% (0.35*1.18*(1000/36.46) = 11.32M

11.97/11.32 = 1.057

Use 5.7% more of the HCI 35% to complete molar ratio?

 

[G.Patton]

You can calculate it easier:
3250g * 0.37 = 1202.5 g of pure HCl in the solution. You have to take same amount of pure HCl in 35% solution.
Hence:
1202.5 g / 0.35 = 3435.7g of 35% HCl solution.

 

[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.