反应详情

To a solution of Example 89E (1.0 g, 5.6 mmol) in THF (30 mL) were added 5-chloro-2-methoxy-benzoic acid (1.86 g, 10.0 mmol, Aldrich), N-(3-dimethylaminopropyl)-N-ethylcarbodimide hydrochloride (1.91 g, 10.0 mmol, Aldrich), 1-hydroxybenzotriazole (1.35 g, 10.0 mmol) and triethylamine (3.5 mL, 3.5 mmol, Aldrich). The mixture was stirred overnight at room temperature. The reaction mixture was then diluted with 1 M aqueous NaHCO3 (20 mL) and the aqueous layer was extracted with ethyl acetate (2×30 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated. The residue was purified by column chromatography (SiO2, 0-5% methanol in dichloromethane to afford 1.55 g (78%) of the title compound. MS (ESI+) m/z 353 (M+H)+

1. extractionthe aqueous layer was extracted with ethyl acetate (2×30 mL)
2. dry with materialThe combined organic extracts were dried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by column chromatography (SiO2, 0-5% methanol in dichloromethane