反应详情

温度

140 °C

To a stirred solution of 6-bromo-3,4-dihydroquinoline-2(1H)-thione (74-4; 1.0 g, 0.004 mol) in n-butanol (20 mL) was added acetic hydrazide (1.19 g, 0.016 mol) at room temperature. Reaction mass was allowed to stir at 140° C. for 5 h. The reaction mixture was cooled to room temperature, diluted with water (50 mL) and extracted with ethyl acetate (3×25 mL). The combined organic layer was washed with saturated aqueous sodium chloride solution, dried over sodium sulphate and concentrated under vacuum to afford the crude compound. Crude compound was purified by silica gel column chromatography to obtain title compound. MS (M+2): 266.0.

1. customReaction mass
2. temperatureThe reaction mixture was cooled to room temperature
3. extractionextracted with ethyl acetate (3×25 mL)
4. washThe combined organic layer was washed with saturated aqueous sodium chloride solution
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated under vacuum
7. customto afford the crude compound
8. customCrude compound was purified by silica gel column chromatography