反应详情

Dissolve the 1-hydroxybenzotriazole hydrate (139 mg, 1.03 mmol), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (197 mg, 1.03 mmol) and 5-dibenzylamino-4-fluoro-isophthalic acid 3-ethyl ester (381 mg, 0.934 mmol) in dichloromethane (10.0 mL). Stir for 30 min. Add methylpropyl amine (68.3 mg, 0.93 mmol) to the reaction mixture. Stir the reaction for 4 h. Add 10% aqueous potassium carbonate solution (10 mL). Extract with dichloromethane (2×50 mL). Combine the organic layers, wash with water (20 mL), saturated aqueous sodium chloride (20 mL), dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 40:60 ethyl acetate:hexanes) to give the title compound (279 mg, 65%).

1. stirringStir
2. customthe reaction for 4 h
3. extractionExtract with dichloromethane (2×50 mL)
4. washCombine the organic layers, wash with water (20 mL), saturated aqueous sodium chloride (20 mL)
5. dry with materialdry (magnesium sulfate)
6. concentrationconcentrate
7. custompurify
8. wash(silica gel chromatography, eluting with 40:60 ethyl acetate:hexanes)