HRID2076008
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 5 °C
PROCEDURE
实验过程
1-(4-Chloro-phenyl)-2-oxo-cyclohexyl-acetonitrile (100 mg, 0.40 mmol) was dissolved in chloroform (1 mL). To this solution bromine (67.7 mg, 0.42 mmol) in chloroform (0.5 mL) was added drop wise at −11° C. The reaction was stirred for 1½ hours at 5° C., then for 1 hours t room temperature and finally for 1 hour at 50° C. The solvent was removed under reduced pressure and the residue was purified by column chromatography on silica gel using dichloromethane as eluent to yield the title compound (104 mg, 79%) as colourless oil. NMR (CDCl3, 300 MHz): δ (ppm)=7.44 (d, 2H), 7.13 (d, 2H), 4.62 (dd, 1H), 2.99 (m, 2.80 (s, 2H), 2.58 (m, 1H), 2.14 (m, 1H), 1.92 (m, 3H).
WORKUP
后处理
- waitfinally for 1 hour at 50° C
- customThe solvent was removed under reduced pressure
- customthe residue was purified by column chromatography on silica gel