反应详情

温度

125 °C

10-Amino-7-fluoro-2-methyl-2,4-dihydro-1,2,3-triazolo[4,5-b][1,5]benzodiazepine hydrochloride (2.68 g) was added to a mixture of dry dimethyl sulphoxide (10 ml), toluene (10 ml) and dry N-methyl piperazine (3.3 ml), which had been degassed with nitrogen for 20 minutes. The stirred solution was then heated at 125° C. (oil-bath) under nitrogen for five hours, cooled to room temperature, and distilled water (33.3 ml) added, keeping the temperature below 25° C. After stirring at 5° C. for half an hour, the suspension obtained was filtered off and dried at 70° C. under reduced pressure to leave a yellow crystalline solid, which was recrystallised from ethyl acetate/n hexane, melting point 195°-197° C.

1. customhad been degassed with nitrogen for 20 minutes
2. temperaturecooled to room temperature
3. distillationdistilled water (33.3 ml)
4. additionadded
5. customthe temperature below 25° C
6. customthe suspension obtained
7. filtrationwas filtered off
8. customdried at 70° C. under reduced pressure
9. customto leave a yellow crystalline solid, which
10. customwas recrystallised from ethyl acetate/n hexane, melting point 195°-197° C.