反应详情

To 3.0 g (0.01 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-oxazepino[6,7-b]-quinolin-5(4H)-one in 30 ml of acetonitrile was added 1.3 g (0.006 mole) of phosphorus pentasulfide. The mixture was stirred vigorously at reflux for 2 hr. After cooling, the reaction mixture was diluted with 60 ml of toluene and filtered. The residue on the filter paper was washed with 50 ml of additional toluene/acetonitrile, 3/1, V/V. The filtrate was washed with 3×50 ml saturated sodium carbonate (caution: gas evolved), dried over anhydrous sodium sulfate, filtered, treated with activated charcoal, filtered again and concentrated by rotary evaporation (90° C., 30 mm). The residual syrup was crystallized from isopropyl alcohol, yielding 1.6 g (52%) of yellow crystals, m.p. 114°-116° C.

1. temperatureat reflux for 2 hr
2. temperatureAfter cooling
3. filtrationfiltered
4. washThe residue on the filter paper was washed with 50 ml of additional toluene/acetonitrile, 3/1, V/V
5. washThe filtrate was washed with 3×50 ml saturated sodium carbonate (caution: gas evolved)
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. additiontreated with activated charcoal
9. filtrationfiltered again
10. concentrationconcentrated by rotary evaporation (90° C., 30 mm)
11. customThe residual syrup was crystallized from isopropyl alcohol