反应详情

温度

5 °C

Dimethylformamide (40 mL) and 40 mL dichloromethane were mixed and cooled to 5° C. Phosphorous oxychloride (37 mL) was dissolved in 40 mL dichloromethane and added dropwise to the dimethylformamide/dichloromethane solution at rate to maintain the temperature below 25° C. Cyclohexanone (10 g, 0.102 mol) was added and the mixture heated at reflux for 3 hours. After cooling to room temperature, the reaction mixture was poured into 200 mL of ice and allowed to sit overnight. The quenched reaction mixture was filtered to collect 3.59 g solid, mp 127° C., λmax =325 nm (ε=14,000).

1. temperatureto maintain the temperature below 25° C
2. temperaturethe mixture heated
3. temperatureat reflux for 3 hours
4. temperatureAfter cooling to room temperature
5. customThe quenched reaction mixture
6. filtrationwas filtered
7. customto collect 3.59 g solid, mp 127° C., λmax =325 nm (ε=14,000)