反应详情

A mixture of 2.0 g of 2-{bis(4-fluorophenyl)hydroxymethyl}-1,3,5-trithiane, 0.2 g of p-toluenesulfonic acid and 50 ml of benzene was refluxed with heating for 15 minutes by means of a Dean-Stark reflux condenser. After being cooled, the mixture was extracted with ethyl acetate and the extract was washed with a saturated aqueous sodium hydrogencarbonate solution. The washed extract was dried over anhydrous magnesium sulfate and the solvent was removed by distillation under reduced pressure to obtain a material, which was recrystalized from cyclohexane to give 1.7 g of the desired compound.

1. temperaturewas refluxed
2. temperaturewith heating for 15 minutes by means of a Dean-Stark
3. temperaturereflux condenser
4. temperatureAfter being cooled
5. extractionthe mixture was extracted with ethyl acetate
6. washthe extract was washed with a saturated aqueous sodium hydrogencarbonate solution
7. extractionThe washed extract
8. dry with materialwas dried over anhydrous magnesium sulfate
9. customthe solvent was removed by distillation under reduced pressure
10. customto obtain a material, which
11. customwas recrystalized from cyclohexane