反应详情

To 1.0 g (0.0039 mole) of 2-(2-chloroethyl)-2,3-dihydro-7-fluoro-4-methyl-1,4-benzoxazepin-5(4H)-one in 30 ml of acetonitrile was added 0.7 g (0.0016 mole) of phosphorus pentasulfide and the reaction mixture heated to reflux. After 2 hr, another 0.4 g (0.009 mole) of phosphorus pentasulfide was added and heating continued for 2 hr. The reaction mixture was diluted with 70 ml of toluene and filtered. The filtrate was washed carefully with 3×50 ml of saturated sodium bicarbonate and 50 ml of water, dried over sodium sulfate, filtered, charcoaled, filtered and concentrated by rotary evaporation. The crude material was recrystallized from diisopropyl ether to give 0.55 g (52%) of yellow crystals, m.p. 135°-137° C.

1. temperaturethe reaction mixture heated to reflux
2. temperatureheating
3. waitcontinued for 2 hr
4. filtrationfiltered
5. washThe filtrate was washed carefully with 3×50 ml of saturated sodium bicarbonate and 50 ml of water
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. filtrationfiltered
9. concentrationconcentrated by rotary evaporation
10. customThe crude material was recrystallized from diisopropyl ether