反应详情

The product of Example 32 (2.6 g, 9 mmol) was dissolved in dichloromethane, the mixture was cooled in an ice-water bath, then N, N-dimethylformamide (2 drops) was added and thionyl chloride (0.64 mL, 10 mmol) was added dropwise, after the addition was complete, the reaction was conducted under reflux for 6 hours and quenched by adding water. After the reaction solution was separated, the aqueous phase was extracted with dichloromethane three times, and the organic phases were combined, washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated to give the target compound 2.4 g, yield: 90%.

1. temperaturethe mixture was cooled in an ice-water bath
2. additionafter the addition
3. temperatureunder reflux for 6 hours
4. customquenched
5. additionby adding water
6. customAfter the reaction solution was separated
7. extractionthe aqueous phase was extracted with dichloromethane three times
8. washwashed with saturated brine
9. dry with materialdried over anhydrous sodium sulfate
10. concentrationconcentrated