反应 #81410

ord-ea54b1f13fea410ab51f39809f353352

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他Prepared in analogy with a method in Hussey
  2. 2
    其他To a 500 mL round-bottomed flask equipped with nitrogen inlet
  3. 3
    其他The organic layer was separated
  4. 4
    洗涤washed again with saturated aqueous sodium bicarbonate solution
  5. 5
    干燥dried over sodium sulfate
  6. 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05618811uspto-grants-1997_04