反应详情

A 2-1, four-necked, round-bottomed flask equipped with stirrer, addition funnel, thermometer and reflux condenser, is charged with 728 g (2 mol) of dried perfluoroheptanoic acid, 160 g (5 mol) of methanol. The mixture is stirred and added dropwise 50 ml concentrated sulfuric acid and then heated to reflux for 4 hr. At the end of the reflux period the mixture is cooled to room temperature and poured into 2 l cold water. After separation of the phases, the lower organic phase is washed with water till pH neutral and dried over CaCl2. Distillation of the crude gives 658 g (87%) of methyl perfluoroheptanoate, bp 139° C.

1. customA 2-1, four-necked, round-bottomed flask equipped with stirrer, addition funnel
2. temperaturethermometer and reflux condenser
3. temperatureheated
4. temperatureto reflux for 4 hr
5. customAfter separation of the phases
6. washthe lower organic phase is washed with water till pH neutral and
7. dry with materialdried over CaCl2
8. distillationDistillation of the crude