反应详情

7-[[(7R)-8-Cyclopentyl-7-ethyl-5-methyl-6-oxo-7H-pteridin-2-yl]amino]-2,2-dimethyl-3H-benzofuran-4-carboxylic acid 4f (116 mg, 0.25 mmol) was dissolved in 15 mL of dichloromethane followed by the addition of (cis)-4-[4-(cyclopropylmethyl)piperazin-1-yl]cyclohexanamine 12e (65 mg, 0.28 mmol), O-(benzotriazol-1-yl)-N,N,N′,N′-tetra methyluronium tetrafluoroborate (80 mg, 0.25 mmol) and diisopropylethylamine (97 mg, 0.75 mmol). The reaction solution was stirred for 3 hours. The resulting solution was added with 20 mL of saturated sodium bicarbonate solution and extracted with dichloromethane (50 mL×3). The combined organic phase was washed with water (50 mL), saturated sodium chloride solution (50 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 to obtain the title compound 7-[[(7R)-8-cyclopentyl-7-ethyl-5-methyl-6-oxo-7H-pteridin-2-yl]amino]-N-[(cis)-4-[4-(cyclopropylmethyl)piperazin-1-yl]cyclohexyl]-2,2-dimethyl-3H-benzofuran-4-carboxamide 23 (135 mg, yield: 78.9%) as a white solid.

1. extractionextracted with dichloromethane (50 mL×3)
2. washThe combined organic phase was washed with water (50 mL), saturated sodium chloride solution (50 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