反应详情

To 30 ml of acetonitrile was added 1.25 g (0.004 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-7-(trifluoromethyl)-1,4-benzoxazepine-5(4H)-one and 0.92 g (0.002 mole) of phosphorus pentasulfide and the reaction mixture heated to reflux for 4 hr. After cooling, 30-40 ml of toluene was added and the mixture filtered. The filtrate was washed with 3×50 ml of saturated potassium carbonate, charcoaled, filtered, and concentrated by rotary evaporation. The residue was crystallized from isopropyl ether to give 0.65 g (50%) of yellow, analytically pure crystals, m.p., 146°-48° C.

1. temperaturethe reaction mixture heated
2. temperatureto reflux for 4 hr
3. temperatureAfter cooling
4. filtrationthe mixture filtered
5. washThe filtrate was washed with 3×50 ml of saturated potassium carbonate
6. filtrationfiltered
7. concentrationconcentrated by rotary evaporation
8. customThe residue was crystallized from isopropyl ether
9. customto give 0.65 g (50%) of yellow, analytically pure crystals
10. customm.p., 146°-48° C.