反应详情

4.7 g of the crude product of example 2a were dissolved in 90 ml of dichloromethane. To this mixture 5.4 ml of chloro sulfonic acid were added drop by drop under stirring at room temperature. The reaction mixture was heated at 50° C. for 1 hour and, after cooling to room temperature, triturated with 70 ml of ice water. After separating the organic layer was dried over sodium sulfate and evaporated to dryness yielding 4.4 g of the crude product.

1. temperatureThe reaction mixture was heated at 50° C. for 1 hour
2. temperatureafter cooling to room temperature
3. customtriturated with 70 ml of ice water
4. customAfter separating the organic layer
5. dry with materialwas dried over sodium sulfate
6. customevaporated to dryness