反应详情

In 500 ml of dichloromethane was dissolved 17.8 g of pentamethylbenzene and the solution was cooled to -5°~-10° C. A solution of 24 ml of chlorosulfonic acid in 400 ml of dichloromethane was added dropwise, and the mixture was allowed to stand at room temperature. The reaction mixture was poured into ice-5% aqueous sodium hydrogen carbonate. The organic layer was washed with water and dried over magnesium sulfate. Removal of the solvent by distillation leaves crystals which were collected by filtration and recrystallized from n-hexane. Yield 27.7 g (93.5%), m.p. 80°-81° C.

1. temperaturethe solution was cooled to -5°~-10° C
2. customto stand at room temperature
3. washThe organic layer was washed with water
4. dry with materialdried over magnesium sulfate
5. customRemoval of the solvent
6. distillationby distillation
7. customleaves crystals which
8. filtrationwere collected by filtration
9. customrecrystallized from n-hexane