反应详情

0.45 g of 4-fluorobenzoic acid (3.21 mmol) and 0.98 g of triethylamine (9.7 mmol) were dissolved in 30 ml of dimethylformamide. At room temperature, 0.5 g of hydroxybenzotriazole (HOBt, 3.7 mmol), 1.2 g of 4-[4-(2-tert-butyl-6-cyclobutyl-pyrimidin-4-yl)-piperazin-1-yl]-butylamine (3.47 mmol), and 0.7 g of N-ethyl-N′-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDCl, 3.65 mmol) were added and the mixture was stirred for 68 h. The reaction mixture was partitioned between water and ethyl acetate. The organic phase was dried over magnesium sulfate, filtered, and concentrated to dryness. The crude product was purified by chromatography on silica gel using dichloromethane-methanol (2%). The oily residue was re-dissolved in isopropanol and 1 N hydrochloric acid in diisopropyl ether was added. The resulting precipitate was filtered and dried to yield 1.2 g of the title compound.

1. customThe reaction mixture was partitioned between water and ethyl acetate
2. dry with materialThe organic phase was dried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated to dryness
5. customThe crude product was purified by chromatography on silica gel
6. dissolutionThe oily residue was re-dissolved in isopropanol
7. addition1 N hydrochloric acid in diisopropyl ether was added
8. filtrationThe resulting precipitate was filtered
9. customdried