反应详情

温度

70 °C

Dissolve 4-chloro-N-(1-phenyl-cyclohexyl)-butyramide (Preparation 29) (0.15 g, 0.53 mmol) in THF (20 mL) and add NaH (0.21 g, 5.29 mmol. 65% wt). Stir and heat the reaction mixture to 70° C. under nitrogen. Continue to heat the reaction at 70° C. for over night then cool it to room temperature. Add water (20 mL), and extract the aqueous layer with dichloromethane (3×50 mL). Combine the organic layers and dry with Na2SO4, filter, concentrate and purify by flash column chromatography (silica gel, 10-40% of EtOAc/Hexane) to give 0.16 g (89%) of the title compound as a colorless oil: Mass spectrum (ion spray): m/z=243.9 (M+).

1. temperatureto heat
2. customthe reaction at 70° C. for over night
3. temperaturethen cool it to room temperature
4. extractionAdd water (20 mL), and extract the aqueous layer with dichloromethane (3×50 mL)
5. dry with materialCombine the organic layers and dry with Na2SO4
6. filtrationfilter
7. concentrationconcentrate
8. custompurify by flash column chromatography (silica gel, 10-40% of EtOAc/Hexane)