反应详情

Phosphorus oxychloride (4.08 mL) was added to cooled (−10° C.) N,N-dimethylformamide (20 mL). The temperature was maintained below 0° C. Stirring was continued for another 30 minutes before the addition of 4-(tert-butyldimethylsilyloxy)cyclohexanone (10 g). The mixture was then stirred at room temperature for 2 hours before it was diluted with ethyl acetate (300 mL) and washed with water (3×), brine and dried over Na2SO4. After filtration and concentration, the crude product was used directly in the next reaction without further purification.

1. temperatureThe temperature was maintained below 0° C
2. stirringThe mixture was then stirred at room temperature for 2 hours before it
3. washwashed with water (3×), brine
4. dry with materialdried over Na2SO4
5. filtrationAfter filtration and concentration
6. customthe crude product was used directly in the next reaction without further purification