반응 #81410

반응 방정식

4-(2-methylphenyl)cyclohexanone

sulfuryl chloride

sodium bicarbonate

→

2-Chloro-4-(2-methylphenyl)cyclohexanone

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   기타Prepared in analogy with a method in Hussey
2. 2
   기타To a 500 mL round-bottomed flask equipped with nitrogen inlet
3. 3
   기타The organic layer was separated
4. 4
   세척washed again with saturated aqueous sodium bicarbonate solution
5. 5
   건조dried over sodium sulfate
6. 6
   기타evaporated to a yellow oil, 41 grams (100%), as a mixture of diastereomers which

실험 절차

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.

출처