pbenz0o
Matrice Périnatale
- Inscrit
- 29/8/07
- Messages
- 12
Hi all,
I've tried out a few times (3 times actually) to make my own MDP2P from safrole using the Dr. Drool method. I bought some nice and rather expensive equipment, reviewed my high school chem lessons and started.
The described method is the Wacker oxydation process using pbenzoquinone / PdCl2 in methanol. I managed to get some really messy crap, but I couldn't get my MDP2P. First time I tried, I left my pbenzo/methanol/safrole/PdCl2 mixture stirring for 8h refluxing methanol (temp 65°C). The result was that, after DCM extraction, the NaOH wash made a really nasty, impossible to separate "mayonnaise". I tried to ditill my MDP2P, but I got apprx half of my safrole back. Next time I tried without applying any heat, same shit.
Has anyone tried this method successfully? I would like to try with DMF instead of methanol, but DMF is really hard to get for me. Next time I'll try the KRV / CuCl2 method...
Thanx
I've tried out a few times (3 times actually) to make my own MDP2P from safrole using the Dr. Drool method. I bought some nice and rather expensive equipment, reviewed my high school chem lessons and started.
The described method is the Wacker oxydation process using pbenzoquinone / PdCl2 in methanol. I managed to get some really messy crap, but I couldn't get my MDP2P. First time I tried, I left my pbenzo/methanol/safrole/PdCl2 mixture stirring for 8h refluxing methanol (temp 65°C). The result was that, after DCM extraction, the NaOH wash made a really nasty, impossible to separate "mayonnaise". I tried to ditill my MDP2P, but I got apprx half of my safrole back. Next time I tried without applying any heat, same shit.
Has anyone tried this method successfully? I would like to try with DMF instead of methanol, but DMF is really hard to get for me. Next time I'll try the KRV / CuCl2 method...
Thanx
