反应详情

温度

35 °C

To a suspension of 33i (Example 14) (0.4 g, 1.22 mmol) in dry DMF (5 ml) is added sodium hydride (50 mg of a 60% dispersion in mineral oil). The mixture is stirred at 30-40° C. for 30 min. 2-Bromopropane (0.14 ml, 1.49 mmol) is added and the mixture is stirred at 40° C. over night. After cooling the mixture is diluted with 4 volumes of water and extracted with dichloromethane. The organic extract is concentrated and eluted through silica gel with ethyl acetate to yield 0.15 g 33j (33%). Mp 77-80° C.

1. stirringthe mixture is stirred at 40° C. over night
2. temperatureAfter cooling the mixture
3. extractionextracted with dichloromethane
4. extractionThe organic extract
5. concentrationis concentrated
6. washeluted through silica gel with ethyl acetate