Oxidative cleavage of piperine to piperonal by ozonolysis

[halohydrin]

After the great safrole drought, many other precursor and synthesis methods appeared. This is one of them starting from piperine (extracted from black pepper). Personally I regard this as the easiest source for MDMA precursor. But it has some impurities in the product and uses ozone generator as oxidizer source - which uses electricity lot.
General Procedure :
1, Piperine solution is prepared by dissolving piperine in 5% solution of water in acetone.
2, Ozone generator is turned on and stream is passed through the solution of 1.
3, After hours passed, the ozone generator is turned off and the solution is extracted with ether 2 times.
4, the combined ether extracts were dried over anhydrous NaSO4 and ether is removed by distillation.
5, remaining oil solidifies by cooling.

The most important part of the reaction is reaction time. One could use higher efficiency ozone generator and even-gas bubbler to make reaction surface larger.
The batch size is the one determines reaction time. On the smaller batches I did(about 1~2 g of piperine), I let the reaction continues overnight - about 8~10 hrs and the all piperine was converted(checked by TLC and GC/MS). I didn't checked the convertion rate mid-reaction, so the reaction might have ended earlier.
I have no experience with larger operations so I can't determine the reaction time for it. But I'm sure It'll need more reaction time due to larger amount of piperine present.

The impurities of the product are different cleavege products at different carbon bonds. But piperonal is the most dominat one. - about 80%.
The separating process is quite difficult since the solubility and composition of the impurities and piperonal are similar. Fractional distillation or precise column chromatography would help.

 

[Sneaky.Base]

Ozonolysis of piperine to piperonal, thats what i m looking for for a while, but full detailed, i read an article sci im sure you too,
Did you done the reaction? Not theory
Or another way to piperonal from piperic acid (oxidation with kmno4 without potassium periodate)?

 

[Macondor]

After the great safrole drought, many other precursor and synthesis methods appeared. This is one of them starting from piperine (extracted from black pepper). Personally I regard this as the easiest source for MDMA precursor. But it has some impurities in the product and uses ozone generator as oxidizer source - which uses electricity lot.
General Procedure :
1, Piperine solution is prepared by dissolving piperine in 5% solution of water in acetone.
2, Ozone generator is turned on and stream is passed through the solution of 1.
3, After hours passed, the ozone generator is turned off and the solution is extracted with ether 2 times.
4, the combined ether extracts were dried over anhydrous NaSO4 and ether is removed by distillation.
5, remaining oil solidifies by cooling.

The most important part of the reaction is reaction time. One could use higher efficiency ozone generator and even-gas bubbler to make reaction surface larger.
The batch size is the one determines reaction time. On the smaller batches I did(about 1~2 g of piperine), I let the reaction continues overnight - about 8~10 hrs and the all piperine was converted(checked by TLC and GC/MS). I didn't checked the convertion rate mid-reaction, so the reaction might have ended earlier.
I have no experience with larger operations so I can't determine the reaction time for it. But I'm sure It'll need more reaction time due to larger amount of piperine present.

The impurities of the product are different cleavege products at different carbon bonds. But piperonal is the most dominat one. - about 80%.
The separating process is quite difficult since the solubility and composition of the impurities and piperonal are similar. Fractional distillation or precise column chromatography would help.

halohydrinUse a lot of Electricity? maybe to convert 100 kg of piperine.
I think with a 10grams per hour generator injecting oxygen can lead to 50 grams per hour of ozone. and can clavage 500 grams of piperine in 8 hours

 

[Sneaky.Base]

Yes it works well and a powerful ozon generator is the key to make this rout worthy.

 

[Macondor]

i only want to know if can make more concetrade , like 100 grm of piperine in 500ml because ..is a pain in the ass or too much volume of solvent to use.. or at less 500 g in 10 liters of acetone.