反应详情

To 7.0 g (0.023 mole) of 2-[2-(dimethylamino)ethyl]-2,3-dihydro-4-methyl-7-nitro-1,4-benzoxazepine-5(4H)-thione was added 250 ml of 23% ammonium sulfide in water. Ethyl alcohol was added in amount sufficient to dissolve the starting compound (~50-60 ml). The reaction mixture was heated to reflux for 5 hr. After cooling, the reaction mixture was acidified with concentrated aqueous hydrochloric acid. The ethanol was removed by rotary evaporation at 70° C. The remaining aqueous solution was washed with 3×100 ml of chloroform, filtered, cooled with ice and made slightly basic with sodium hydroxide. The aqueous was then extracted with 3×100 ml of chloroform, dried over sodium sulfate, filtered and concentrated by rotary evaporation. The residue was crystallized from isopropyl alcohol to give 3.5 g (55%) of yellow analytically pure crystals.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 5 hr
3. temperatureAfter cooling
4. customThe ethanol was removed by rotary evaporation at 70° C
5. washThe remaining aqueous solution was washed with 3×100 ml of chloroform
6. filtrationfiltered
7. temperaturecooled with ice
8. extractionThe aqueous was then extracted with 3×100 ml of chloroform
9. dry with materialdried over sodium sulfate
10. filtrationfiltered
11. concentrationconcentrated by rotary evaporation
12. customThe residue was crystallized from isopropyl alcohol
13. customto give 3.5 g (55%) of yellow analytically pure crystals