反应详情

温度

140 °C

(4-Bromophenyl)(6-methoxypyridin-3-yl)methanone (0.88 g, 3.0 mmol), hydrazine monohydrate (1.5 mL, 30 mmol) and potassium hydroxide (0.60 g, 12 mmol) were dissolved in ethylene glycol (10 mL), followed by stirring at 140° C. for 20 minutes. After the reaction solution was cooled to room temperature, water was added, followed by extraction with diethyl ether. After the organic layer was concentrated under reduced pressure, the resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/ethyl acetate), and a fraction corresponding to the Rf value=0.30 (hexane/ethyl acetate=1/1) by thin layer chromatography was concentrated under reduced pressure to afford the title compound (0.38 g, 1.2 mmol) as a colorless oil (yield 41%).

1. temperatureAfter the reaction solution was cooled to room temperature
2. extractionfollowed by extraction with diethyl ether
3. concentrationAfter the organic layer was concentrated under reduced pressure
4. customthe resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/ethyl acetate)
5. concentrationa fraction corresponding to the Rf value=0.30 (hexane/ethyl acetate=1/1) by thin layer chromatography was concentrated under reduced pressure