反应详情

温度

0 °C

Dissolve 4-(cyclohexyl-hydroxy-methyl)-benzonitrile (1 g, 4.66 mmol), and triethylamine (1.3 mL, 9.3 mmol) in dichloromethane (20 mL). Cool the mixture to 0° C., add methanesulfonyl chloride (1.49 mL, 5.34 mmol) and stir the solution for 2 h at 0° C. Add water (10 mL) and saturated aqueous NaHCO3 (10 mL). Separate the layers and extract back the aqueous phase with dichloromethane (3×20 mL). Combine the organic layers, wash with water (20 mL), dry over Na2SO4, filter and concentrate in vacuo to provide the desired intermediate as a yellow oil (1.29 g, 94%). MS (APCI) m/z: 294 (M+H)+.

1. customSeparate the layers
2. extractionextract back the aqueous phase with dichloromethane (3×20 mL)
3. washCombine the organic layers, wash with water (20 mL)
4. dry with materialdry over Na2SO4
5. filtrationfilter
6. concentrationconcentrate in vacuo