反应详情

To a suspension of 11.3 g of 2-trichloroacetamido-5-chlorobenzophenone in 100 ml. of ethanol was added 4.51 g of 3-amino-1-propanol. The mixture was heated under reflux for 3 hours. Then, 1.7 g of potassium hydroxide was added thereto and the resulting mixture was further refluxed for 3 hours. After cooling, the precipitate was filtered off and washed with ethanol. The filtrate was concentrated under reduced pressure and to the residue was added 200 ml. of water. The resulting solid was collected by filtration, washed with water and dried to give 9.87 g of 10-chloro-3,4,7,11b-tetrahydro-11b-phenyl-2H,6H-[1,3]oxazino[3,2-C]quinazolin-6-one. Recrystallization from ethanol gave pale yellow prisms, having a melting point of 202°-203.5°C.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 3 hours
3. temperaturethe resulting mixture was further refluxed for 3 hours
4. temperatureAfter cooling
5. filtrationthe precipitate was filtered off
6. washwashed with ethanol
7. concentrationThe filtrate was concentrated under reduced pressure and to the residue
8. additionwas added 200 ml
9. filtrationThe resulting solid was collected by filtration
10. washwashed with water
11. customdried