суббота, 2 февраля 2013 г.

Synthesis #1: Demethylation veratraldehyde by sulfuric acid

Hello!

One day i see publication: SELECTIVE HYDROLYSIS OF DIALKYL ETHERS OF PROTOCATECHUIC ALDEHYDE
And try to repeat that on practice.

24 g veratraldehyde has  added to 75 ml highly concentrated sulfuric acid. Reaction mass has colored to yellow. Than, to orange.


Finally, R.M. was heated to 120 "С during 10 min and has retentioned during 2,5 hours.
After 10 seconds of heating, R.M. has colored to red, then - to dark green (quinhydrone, I think). Then - to  dark violet. And, finally, to dark red.







Then, I tried to handle the reaction the following way:

                                                                           
R.M. was diluted by 100 ml cold water.
Then, I tried extract anything (solvent:  DCE and DCM) Nothing.












I added  another 260 ml water and left it for night. On the morning, I saw big amount of coated black resin.


P.S. Sorry for my bad English.

Best regards, Sergey.