反应详情

To a solution of the compound (168 mg) obtained in Step 2 in N,N-dimethylformamide (1.7 ml) were successively added, with stirring under ice-cooling, 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (94 mg), 1-hydroxybenzotriazole hydrate (75 mg) and 4-trifluoromethoxybenzylamine (85 mg). After stirring overnight at room temperature, the mixture was partitioned by adding ethyl acetate, saturated aqueous sodium hydrogen carbonate solution and water. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure. The residue was purified by thin layer silica gel chromatography (hexane:ethyl acetate=1:1) to give the title compound (132 mg).

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