反应 #81410
ord-ea54b1f13fea410ab51f39809f353352
反应方程式
反应条件
后处理
- 1其他Prepared in analogy with a method in Hussey
- 2其他To a 500 mL round-bottomed flask equipped with nitrogen inlet
- 3其他The organic layer was separated
- 4洗涤washed again with saturated aqueous sodium bicarbonate solution
- 5干燥dried over sodium sulfate
- 6其他evaporated to a yellow oil, 41 grams (100%), as a mixture of diastereomers which
实验过程
Prepared in analogy with a method in Hussey, A. S. and Herr, R. R., J. Org. Chem., 24, 843 (1959). To a 500 mL round-bottomed flask equipped with nitrogen inlet were added 33.3 grams (0.177 tool) of 4-(2-methylphenyl)cyclohexanone and 200 mL methylene chloride. To the stirring solution was added dropwise over 30 minutes a solution of 17.1 mL (0.212 mol) sulfuryl chloride in 10 mL methylene chloride. The reaction was stirred 14 hours at room temperature and poured into saturated aqueous sodium bicarbonate solution. The organic layer was separated, washed again with saturated aqueous sodium bicarbonate solution, dried over sodium sulfate, and evaporated to a yellow oil, 41 grams (100%), as a mixture of diastereomers which was used directly in the next step.