反应详情

Under an argon atmosphere, triethylamine (0.028 ml) and 2,6-difluorobenzoyl chloride (0.015 ml) were added to a solution of 2-amino-5-[4-(methyl-pyrimidin-2-ylamino)phenyl]pent-4-enoic acid methyl ester (31.7 mg) in dichloromethane (2 ml), and the resulting mixture was stirred at room temperature for 2 hours. Saturated aqueous sodium hydrogen carbonate solution was added to the reaction solution and the resulting mixture was extracted with ethyl acetate. Organic layer was washed twice with water and once with saturated brine, and dried over anhydrous sodium sulfate. After removing anhydrous sodium sulfate by filtration, the filtrate was concentrated. The residue was purified by thin layer chromatography (silica gel, developing solvent: cyclohexane/ethyl acetate=3/2) to obtain (E)-2-(2,6-difluorobenzamido)-5-[4-(methyl-pyrimidin-2-ylamino)phenyl]pent-4-enoic acid methyl ester (42 mg).

1. extractionthe resulting mixture was extracted with ethyl acetate
2. washOrganic layer was washed twice with water and once with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. customAfter removing anhydrous sodium sulfate
5. filtrationby filtration
6. concentrationthe filtrate was concentrated
7. customThe residue was purified by thin layer chromatography (silica gel, developing solvent: cyclohexane/ethyl acetate=3/2)