反应详情

To a solution of 204 mg of 4-((6-((1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazol-3-yl)amino)pyridin-2-yl)methyl)piperidin-4-ol in 10 ml of chloroform were added 132 mg of 3-chloro-2-fluorobenzoic acid, 116 mg of hydroxybenzotriazole hydrate and 194 mg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride at room temperature, followed by stirring the reaction mixture at room temperature overnight. The reaction mixture was poured into saturated aqueous sodium bicarbonate solution, and extracted with chloroform. The resulting chloroform layer was dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated in vacuo. The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=10/1 to ethyl acetate) to give the title compound as a colorless oil.

1. extractionextracted with chloroform
2. dry with materialThe resulting chloroform layer was dried over anhydrous magnesium sulfate
3. filtrationfiltered
4. concentrationThe filtrate was concentrated in vacuo
5. customThe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=10/1 to ethyl acetate)