反应详情

温度

85 °C

A mixture of 2.00 g (5.20 mmol) of the starting material I, 1.89 g (10.44 mmol) of ethyl 3-bromopropionate and 20 ml of dimethylformamide was stirred at 80-90° C. for 3 h. The reaction mixture was diluted with 25% sodium chloride solution and extracted with dichloromethane. After drying and concentration the crude product was purified by column chromatography using silica gel (MN Kieselgel 60) as adsorbent and a mixture of ethyl acetate-methanol (2:1) as eluent to yield 1.34 g (59%) of the title compound; Mp.: 220-221° C.

1. extractionextracted with dichloromethane
2. customAfter drying
3. concentrationconcentration the crude product
4. customwas purified by column chromatography
5. additiona mixture of ethyl acetate-methanol (2:1) as eluent