反应详情

To a solution of the compound obtained in stage A (15 g, 79 mmol) in EtOH (500 ml) was added dropwise SOCl2 (40 mL). The resulting mixture was stirred under reflux during 12 hours. After adding water (200 mL), the pH was adjusted to 7.0 with 20% aqueous Na2CO3. The aqueous solution was extracted with CH2Cl2 (3×200 mL). The combined organic layers were dried over MgSO4, filtered and evaporated to afford 11 g (yield: 64%) of the product of molecular formula C12H11NO3. Aspect: pale brown powder.

1. temperatureunder reflux during 12 hours
2. extractionThe aqueous solution was extracted with CH2Cl2 (3×200 mL)
3. dry with materialThe combined organic layers were dried over MgSO4
4. filtrationfiltered
5. customevaporated