反应详情

温度

25 °C

A solution containing the product from Example 10A (1.76 g, 5.25 mmol) in 1,2-dichloroethane (210 mL) was treated with N,N-disuccinimidyl carbonate (1.61 g, 6.28 mmol) and triethylamine (0.75 mL, 5.38 mmol), stirred at 25° C. for 16 hours, and partitioned with 10% Na2CO3. The aqueous phase was extracted with additional dichloromethane. The combined organic phase was dried over MgSO4, filtered and concentrated. The residue was chromatographed on silica gel eluting with 0-25% methyl tert-butyl ether/dichloromethane to give the title compound (1.33 g, 70% yield).

1. custompartitioned with 10% Na2CO3
2. extractionThe aqueous phase was extracted with additional dichloromethane
3. dry with materialThe combined organic phase was dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was chromatographed on silica gel eluting with 0-25% methyl tert-butyl ether/dichloromethane