反应详情

To 2.0 g (0.007 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-7-nitro-1,4-benzoxazepin-5(4H)-one in 35 ml of acetonitrile was added 1.0 g (0.0023 mole) of phosphorus pentasulfide and the mixture heated to reflux for 2 hr. Another 0.4 g (0.001 mole) of phosphorus pentasulfide was added and heating continued for 2 hr. After cooling, the reaction mixture was diluted with 100 ml of toluene and filtered. The filtrate was washed with 3×50 ml of saturated sodium bicarbonate and 100 ml of water, dried over sodium sulfate, filtered, charcoaled, filtered, and concentrated by rotary evaporation. The crude oil was crystallized from isopropyl ether/toluene to give 1.2 g (57%) of yellow crystals, m.p. 153°-155° C.

1. temperaturethe mixture heated
2. temperatureto reflux for 2 hr
3. temperatureheating
4. temperatureAfter cooling
5. filtrationfiltered
6. washThe filtrate was washed with 3×50 ml of saturated sodium bicarbonate and 100 ml of water
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. filtrationfiltered
10. concentrationconcentrated by rotary evaporation
11. customThe crude oil was crystallized from isopropyl ether/toluene