反应详情

2,3-dimethylbenzothiazolinium-p-toluene sulphonate (10 g) was slurried in dry toluene (50 ml) and cooled to 5 degC. A solution of 4-trichloromethylbenzoyl chloride (8.9 g) in dry toluene (10 ml) was added dropwise to the stirred slurry over a period of 30 minutes, maintaining the temperature at 10-15 degC. A solution of triethylamine (7 ml) in dry toluene (10 ml) was then added dropwise over a period of 30 minutes, the temperature again being maintained at 10-15 degC. The reaction mixture was stirred for two hours at room temperature. The solid product was filtered off, reslurried in methanol and recrystallised from a 3/1 chloroform/methanol solution.

1. temperaturecooled to 5 degC
2. temperaturemaintaining the temperature at 10-15 degC
3. temperaturethe temperature again being maintained at 10-15 degC
4. filtrationThe solid product was filtered off
5. customrecrystallised from a 3/1 chloroform/methanol solution