反应详情

Under an argon atmosphere, EDC hydrochloride (39 mg) and HOBT (3 mg) were added to a solution of 2-amino-5-[4-(methyl-pyrimidin-2-ylamino)phenyl]pent-4-enoic acid methyl ester (51 mg) and 2-chloro-6-fluorobenzoic acid in dichloromethane (1.5 ml), and the resulting mixture was stirred at room temperature for 28 hours. To the reaction solution, 1N hydrochloric acid was added, and the resulting mixture was extracted with ethyl acetate. Organic layer was washed with saturated aqueous sodium hydrogen carbonate solution 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, mobile phase: hexane/ethyl acetate=1/2) to obtain (E)-2-(2-chloro-6-fluorobenzamido)-5-[4-(methyl-pyrimidin-2-ylamino)phenyl]pent-4-enoic acid methyl ester (39 mg).

1. extractionthe resulting mixture was extracted with ethyl acetate
2. washOrganic layer was washed with saturated aqueous sodium hydrogen carbonate solution
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, mobile phase: hexane/ethyl acetate=1/2)