反应详情

A mixture of 18.5 g (0.0834 mole) of phosphorus pentasulfide and 18.5 g potassium sulfide was ground together and added to a solution of 100 g (0.417 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in dry toluene, the mixture refluxed 24 hr. and filtered. The filtrate was concentrated and partitioned between chloroform and dilute sodium hydroxide. The chloroform layer was concentrated and the residue was crystallized several times from ethanol. Yield of product was 55 g (52%), m.p. 105°-108° C.

1. temperaturethe mixture refluxed 24 hr
2. filtrationand filtered
3. concentrationThe filtrate was concentrated
4. custompartitioned between chloroform and dilute sodium hydroxide
5. concentrationThe chloroform layer was concentrated
6. customthe residue was crystallized several times from ethanol