反应详情

温度

-10 °C

Into a 250 mL round-bottomed flask was added N,N-dimethylformamide (3.5 mL) in dichloromethane (30 mL) to give a colorless solution. The mixture was cooled to −10° C., and phosphoryl trichloride (4 mL) was added dropwise. The solution was warmed up to room temperature, and 3,3-dimethylcyclohexanone (5.5 mL) was added slowly. The mixture was heated to reflux for overnight. The reaction mixture was quenched by 0° C. solution of sodium acetate (25 g in 50 mL water). The aqueous layer was extracted with ether (3×200 mL). The organic layers were combined, dried over Na2SO4, filtered, and dried under vacuum.

1. customto give a colorless solution
2. temperatureThe solution was warmed up to room temperature
3. temperatureThe mixture was heated
4. temperatureto reflux for overnight
5. customThe reaction mixture was quenched by 0° C. solution of sodium acetate (25 g in 50 mL water)
6. extractionThe aqueous layer was extracted with ether (3×200 mL)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. customdried under vacuum