反应详情

To a solution of the compound (1.24 g) obtained in Example 1001, Step 1 in N,N-dimethylformamide (12 ml) were added, with stirring under ice-cooling, 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (0.65 g), 1-hydroxybenzotriazole hydrate (0.52 g) and the compound (0.59 g) obtained in Step 3. After stirring overnight at room temperature, the reaction mixture was partitioned by adding saturated aqueous sodium hydrogen carbonate solution and ethyl acetate. The organic layer was washed successively with water and saturated brine, dried over anhydrous sodium sulfate, filtrated, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (methanol:chloroform=4:96-6:94) to give the title compound (1.70 g).

1. temperaturecooling
2. stirringAfter stirring overnight at room temperature
3. customthe reaction mixture was partitioned
4. additionby adding saturated aqueous sodium hydrogen carbonate solution and ethyl acetate
5. washThe organic layer was washed successively with water and saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltrated
8. concentrationconcentrated under reduced pressure
9. customThe residue was purified by silica gel column chromatography (methanol:chloroform=4:96-6:94)