反应详情

In 500 ml of methylene chloride was dissolved 4.5 g of 2,3,5-trimethylanisole and the solution was cooled to -5° C. to -10° C. A solution of 6.0 ml of chlorosulfonic acid in 400 ml of methylene chloride was added dropwise, and then the temperature was allowed to rise to room temperature. The mixture was poured into an ice--5% aqueous sodium hydrogen carbonate mixture. The methylene chloride layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was then distilled off, and the residue was crystallized from n-hexane.

1. temperaturethe solution was cooled to -5° C. to -10° C
2. customto rise to room temperature
3. washThe methylene chloride layer was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationThe solvent was then distilled off
6. customthe residue was crystallized from n-hexane