反应详情

温度

60 °C

To a stirred solution of 1-(cyclopropyl-hydroxy-methyl)-4-cyclopropylmethylsulfanyl-cyclohexanecarbonitrile (1.93 g; 7.27 mmol) in acetone (15 ml) was added a slurry of oxone (13.4 g; 21.8 mmol) in water (10 ml). The mixture was heated at 60° C. for 1 hour then allowed to cool to room temperature. Water (50 ml) was added and the pH was adjusted to 7 with 2 M sodium carbonate solution. The mixture was extracted with EtOAc (80 ml) and DCM 950 ml). The combined organics were dried (MgSO4) and evaporated in vacuo to give the product as a white solid (1.9015 g). 1H NMR (400 MHz, DMSO): δ 5.36 (1H, d, J 5.0), 3.11-3.05 (3H, m), 2.78 (1H, dd, J 4.8, 7.8), 2.26-2.20 (1H, m), 2.14-2.08 (3H, m), 1.67-1.43 (4H, m), 1.08-0.84 (2H, m), 0.62-0.58 (2H, m), 0.53-0.49 (1H, m), 0.46-0.30 (5H, m). m/z=320 (M+Na+).

1. temperatureto cool to room temperature
2. extractionThe mixture was extracted with EtOAc (80 ml) and DCM 950 ml)
3. dry with materialThe combined organics were dried (MgSO4)
4. customevaporated in vacuo