反应详情

温度

0 °C

To a stirred solution of methyl 2-acetyl-3-(3-cyclopentyloxy-4-methoxyphenyl)-butanoate (362 mg, 1.08 mmol) in absolute ethanol (10 ml) at 0° C. was added hydrazine monohydrate (54 mg, 1.08 mmol) in one portion. The resulting solution was stirred at 0° C. for 45 minutes and then refluxed at 80° C. for 3 hours. Further hydrazine monohydrate (15.6 mg, 3.1×10-4 mol) was added and refluxing continued for a further 3 hours. After cooling to room temperature, the reaction mixture was concentrated in vacuo and purified by flash chromatography (SiO2 ; methylene chloride/ethanol/ammonia (97.5:2.5:0.25)) to afford the title compound as a white solid (76 mg).

1. temperaturerefluxed at 80° C. for 3 hours
2. temperaturerefluxing
3. waitcontinued for a further 3 hours
4. temperatureAfter cooling to room temperature
5. concentrationthe reaction mixture was concentrated in vacuo
6. custompurified by flash chromatography (SiO2 ; methylene chloride/ethanol/ammonia (97.5:2.5:0.25))