反应详情

温度

125 °C

10-Amino-6,7-dichloro-2-methyl-2,4-dihydro-1,2,3-triazolo[4,5-b][1,5]benzodiazepine hydrochloride (0.84 g) was added to a mixture of dry dimethylsulphoxide (5 ml), toluene (5 ml) and N-methylpiperazine (1 ml), which had been purged with nitrogen for 20 minutes. The stirred solution was then heated at 125° C. (oil bath) under nitrogen for 16 hours, cooled to room temperature, and distilled water (10 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-brown solid which was recrystallised from ethyl acetate/n-hexane to give a yellow crystalline solid, melting point 217.5°-218.5° C.

1. customhad been purged with nitrogen for 20 minutes
2. temperaturecooled to room temperature
3. distillationdistilled water (10 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-brown solid which
10. customwas recrystallised from ethyl acetate/n-hexane
11. customto give a yellow crystalline solid, melting point 217.5°-218.5° C.