反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Into a 50 mL round-bottom flask, was placed a solution of tert-butyl 4-(4-(3-methyl-4-oxo-1-phenyl-4,7-dihydro-1H-pyrazolo[3,4-b]pyridin-6-yl)phenyl)piperazine-1-carboxylate (300 mg, 0.62 mmol, 1.00 equiv) in dichloromethane (6 mL), trifluoroacetic acid (3 mL). The resulting solution was stirred for 2 h at room temperature. The resulting mixture was then concentrated under vacuum. The pH value of the solution was adjusted to about 9-10 with sodium bicarbonate. The resulting solution was extracted with of ethyl acetate (2×10 mL), the organic layers combined and dried over anhydrous magnesium sulfate. The residue was applied onto a silica gel column with MeOH:DCM (1:40) to yield 3-methyl-1-phenyl-6-(4-(piperazin-1-yl)phenyl)-1H-pyrazolo[3,4-b]pyridin-4(7H)-one as a yellow solid.
WORKUP
后处理
- customInto a 50 mL round-bottom flask, was placed
- concentrationThe resulting mixture was then concentrated under vacuum
- extractionThe resulting solution was extracted with of ethyl acetate (2×10 mL)
- dry with materialdried over anhydrous magnesium sulfate