反应详情

Dissolve 5-(methyl-propylcarbamoyl)-isophthalic acid monoethyl ester (667 mg, 2.3 mmol) in a 0.1 N 1-hydroxybenzotriazole solution of 1:1:5 tert-butanol:acetonitrile:dichloromethane (23 mL, 2.3 mmol). Stir the solution at room temperature for 5 min, add 3,3-difluoropyrrolidine hydrochloride (331 mg, 2.3 mmol) and triethylamine (640 μL, 4.6 mmol). Stir the reaction at room temperature for 2 h, add ethyl acetate (100 mL) and wash with saturated aqueous ammonium chloride (2×30 mL), saturated aqueous sodium chloride (30 mL), dry (sodium sulfate), concentrate and purify (silica gel chromatography, eluting with 50:50 ethyl acetate:hexanes) to give the title compound (270 mg, 31%).

1. stirringStir
2. customthe reaction at room temperature for 2 h
3. washwash with saturated aqueous ammonium chloride (2×30 mL), saturated aqueous sodium chloride (30 mL)
4. dry with materialdry (sodium sulfate)
5. concentrationconcentrate
6. custompurify
7. wash(silica gel chromatography, eluting with 50:50 ethyl acetate:hexanes)