反应详情

The TLC test indicated that the reaction was not yet complete so another 1 g of paraformaldehyde was added 45 minutes after the first. Heating of the reaction mixture was continued at 125° C. After 1.5 hours total heating, a second TLC sample was taken and analyzed as above and it indicated that the estazolam was almost all consumed. To ensure complete reaction, another 0.5 g of paraformaldehyde was added and heating of the mixture was continued at 125° C. for another 45 minutes (2.25 hours total heating time), at which time testing by TLC analysis indicated reaction was substantially complete to form 1-(hydroxymethyl)-8-chloro-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine.

1. additionwas added 45 minutes after the first
2. temperatureHeating of the reaction mixture
3. customwas continued at 125° C
4. customreaction
5. temperatureheating of the mixture
6. waitwas continued at 125° C. for another 45 minutes
7. custom(2.25 hours total heating time)
8. customreaction