反应详情

温度

100 °C

50.6 g (0.3 mol) of 3,4-dimethylbenzoyl chloride were warmed to 80° C. under a nitrogen atmosphere. 69 g (0.3 mol) of 6-methoxy-(6H)-dibenz[c,e][1,2]oxaphosphorin were added dropwise while stirring. Crystallization began even during the dropwise addition, and the temperature was therefore increased to 100° C.; at the same time, an additional 100 ml of toluene were added dropwise. When the dropwise addition was complete, the mixture was heated to reflux. When the reaction was complete and after crystallization, 87 g (83% of theory) of the abovementioned compound, which had a melting point of 160° to 162° C., were obtained.

1. customCrystallization
2. additionbegan even during the dropwise addition
3. additionat the same time, an additional 100 ml of toluene were added dropwise
4. additionWhen the dropwise addition
5. temperaturethe mixture was heated to reflux
6. customafter crystallization, 87 g (83% of theory) of the abovementioned compound, which
7. customwere obtained