反应详情

A suspension of 1.95 g (4.0 mmoles) of 7-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepin in 10 ml of ethylene glycol containing 4 ml of triethylamine was heated on a steam bath for 2 hrs. A clear solution formed soon after heating began. Triethylamine was removed in vacuo. The ethylene glycol solution was poured into ice water precipitating solids which were collected and washed thoroughly with water. Remaining water was removed from the solid by dissolving in solid in ether, drying over sodium sulfate and evaporation of ether. Crystallization of the residue from ether-hexane gave colorless prisms, mp 142°-144°.

1. temperaturewas heated on a steam bath for 2 hrs
2. customA clear solution formed soon
3. temperatureafter heating
4. customTriethylamine was removed in vacuo
5. additionThe ethylene glycol solution was poured into ice water precipitating solids which
6. customwere collected
7. washwashed thoroughly with water
8. customRemaining water was removed from the solid
9. dissolutionby dissolving in solid in ether
10. dry with materialdrying over sodium sulfate and evaporation of ether
11. customCrystallization of the residue from ether-hexane
12. customgave colorless prisms, mp 142°-144°