反应详情

273 mg of 1-(3-chloro-2-fluorobenzoyl)-4-((6-((1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazol-3-yl)amino)pyridin-2-yl)methyl)piperidin-4-ol was dissolved in 3 ml of trifluoroacetic acid and 0.3 ml of water, followed by stirring the reaction mixture at room temperature for 1.5 hours. The reaction mixture was concentrated in vacuo, basified with saturated aqueous sodium bicarbonate solution, and extracted with ethyl acetate. The resulting ethyl acetate 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: chloroform to chloroform/methanol=10/1). The obtained free form was dissolved in 5 ml of ethyl acetate. 0.5 ml of 4 M hydrogen chloride in 1,4-dioxane was added to the solution at room temperature, followed by diluting with 5 ml of tert-butyl methyl ether. The precipitate was collected and washed with tert-butyl methyl ether to give the title compound as a white solid.

1. concentrationThe reaction mixture was concentrated in vacuo
2. extractionextracted with ethyl acetate
3. dry with materialThe resulting ethyl acetate layer was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated in vacuo
6. customThe resulting residue was purified by a silica gel column chromatography (eluent: chloroform to chloroform/methanol=10/1)
7. dissolutionThe obtained free form was dissolved in 5 ml of ethyl acetate
8. addition0.5 ml of 4 M hydrogen chloride in 1,4-dioxane was added to the solution at room temperature
9. additionby diluting with 5 ml of tert-butyl methyl ether
10. customThe precipitate was collected
11. washwashed with tert-butyl methyl ether