反应详情

To a solution of 97 (3 g, 4.7 mmol) in acetone (16 mL) and water (4 mL) was added CaCO3 (4.7 g, 47 mmol) and CH3I (13.2 g, 94 mmol). After kept 20 hours at 50° C., the resulting solution was diluted with dichloromethane (30 mL), filtered and extracted with dichloromethane (2×30 mL). The combined organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford crude 98, which was used in next step directly; (ES, m/z) [M+H]+ 547.0.

1. filtrationfiltered
2. extractionextracted with dichloromethane (2×30 mL)
3. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customto afford crude 98, which