反应详情

To a solution of the compound (1.35 g) obtained in Example 783, Step 2 in chloroform (15 ml) were added 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (625 mg), 1-hydroxybenzotriazole hydrate (499 mg) and 3-fluoro-4-trifluoromethoxybenzylamine (620 mg) with stirring under ice-cooling. After stirring overnight at room temperature, the reaction mixture was partitioned by adding saturated aqueous sodium hydrogen carbonate solution and chloroform, and the aqueous layer was re-extracted twice with chloroform. The organic layers were combined, dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:l) to give the title compound (1.50 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 chloroform
5. extractionthe aqueous layer was re-extracted twice with chloroform
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltrated
8. concentrationconcentrated under reduced pressure
9. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:l)