反应详情

A mixture of 4-(1,3-dioxoisoindolin-2-yl)cyclohexane-1-sulfonic acid (6.8 g, 22 mmol) and PCl5 (5 g, 24 mmol) was stirred at room temperature for 30 min. And then the mixture was heated at 100° C. and stirred for 2 h. After cooling to room temperature, the mixture was washed with EtOAc (150 mL×3). The combined extracts were concentrated in vacuo to give crude 4-(1,3-dioxoisoindolin-2-yl)cyclohexane-1-sulfonyl chloride (5 g, 68%) as a whit solid, which was used in the next step directly.

1. temperatureAnd then the mixture was heated at 100° C.
2. stirringstirred for 2 h
3. temperatureAfter cooling to room temperature
4. washthe mixture was washed with EtOAc (150 mL×3)
5. concentrationThe combined extracts were concentrated in vacuo