反应详情

温度

50 °C

A solution of 0.30 g (1.3 mmol) of 1-(o-aminophenyl)-4-chloro-1-butanone hydrochloride in 3 mL of methylene chloride and 3 mL of ethylene dichloride is treated with 1.2 g (3 mmol) of 10% sodium hydroxide solution and 0.05 g (0.2 mmol) of 75% aqueous methyl tributylammonium chloride and heated to 50° C. for about 5 hours. After cooling to room temperature, the phases are separated. The aqueous layer is extracted with methylene chloride. The combined organic extracts are washed with water and concentrated in vacuo to give 0.14 g (70% yield) of o-aminophenyl cyclopropyl ketone (mp 46-48° C.). The product is identified by NMR and MS analyses.

1. temperatureAfter cooling to room temperature
2. customthe phases are separated
3. extractionThe aqueous layer is extracted with methylene chloride
4. washThe combined organic extracts are washed with water
5. concentrationconcentrated in vacuo