MDP2P Steam Distillation

[rothschild33]

Have done several steam distillation for MDP2P synthesized from 28578. Tried using a steam generator with 105C steam, adding potassium carbonate to the distillation flask, adjusting the water amount in distillation flask. Also tried adding saturated salt solution to the distilled solution and always extract with DCM. Every time the yield is always 0.5 - 1 ml MDP2P for every 100 ml water distilled. I checked resources online from Hellman's post in mdma.ch, is it really supposed to be 1 ml MDP2P for every 100 ml water distilled?

 

[blackburn]

you should use an extra heat source, in addition to your steam generator

 

[rothschild33]

the distillation flask is heated at 80C in an oil bath in addition to the steam generated externally

 

[blackburn]

More heat,

 

[rothschild33]

hmm, will try this and report back on any change

 

[TheCook]

Hi!

Does it just look like that, or do you have too little oil in the oil bath? It should be as high as the level in the flask. And you have to make sure that it stays that way. This means that if the water level in the flask rises above that of the oil, you have to heat it up sufficiently (set to 130°C might be sufficient). If the water level drops too low, you have to reduce the heat a little.
You must also remember that the set temperature of the magnetic stirrer has nothing to do with the temperature in the flask. You have to set it at least 20°C higher than the temperature you will expect in the flask.
And wrap the entire steam hose in aluminium foil.
Finally, you also have to remember that all the heat you put in has to be dissipated again. Your Liebing cooler looks pretty small. I hope you have a vacuum inlet, connected to a gas washing flask that you've immersed in ice water.

Good luck next time.

 

[OrgUnikum]

You would have to pressurize the whole system to get decent results. Otherwise its 1ml to 100 ml at best.

 

[qwe111]

gentlemen.
Is your steam distillation tuned to perfection?
Can you share it with me? I'm stuck with this problem.

I also use the same pressure cooker as you.

10L pressure cooker. 5L distillation bottle. How much P2P can I distill at a time?

What is the ratio of P2P to potassium carbonate solution?