反应详情

7-[(8-Cyclopentyl-7,7-diethyl-5-methyl-6-oxo-pteridin-2-yl)amino]-2,3-dihydrobenzofuran-4-carboxylic acid 42b (50 mg, 0.11 mmol) was dissolved in 20 mL of dichloromethane followed by the addition of O-(benzotriazol-1-yl)-N,N,N′,N′-tetra methyluronium tetrafluoroborate (35 mg, 0.11 mmol), diisopropylethylamine (31 mg, 0.24 mmol) and 1-methyl-piperidyl-4-yl-amine (13 mg, 0.11 mmol) successively. The reaction solution was stirred at room temperature for 1 hour. The resulting solution was added with 50 mL of saturated sodium carbonate solution and extracted with dichloromethane (100 mL×2). The combined organic phase was washed with water (20 mL) and saturated sodium chloride solution (20 mL) successively, then dried over anhydrous magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography with elution system A to obtain the title compound 7-[(8-cyclopentyl-7,7-diethyl-5-methyl-6-oxo-pteridin-2-yl)amino]-N-(1-methyl-4-piperidyl)-2,3-dihydrobenzofuran-4-carboxamide 42 (10 mg, yield: 16.0%) as a white solid.

1. extractionextracted with dichloromethane (100 mL×2)
2. washThe combined organic phase was washed with water (20 mL) and saturated sodium chloride solution (20 mL) successively
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography with elution system