HRID68742

反应详情

EQUATION

反应方程式

HRID 68742 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 50 mL round-bottom flask, was placed a solution of tert-butyl 4-(4-(3,7-dimethyl-4-oxo-1-phenyl-4,7-dihydro-1H-pyrazolo[3,4-b]pyridin-6-yl)phenyl)piperazine-1-carboxylate (270 mg, 0.54 mmol, 1.00 equiv) in dichloromethane (6 mL), trifluoroacetic acid (3 mL). The resulting solution was stirred overnight at room temperature. The resulting mixture was 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 (3×10 mL), the organic layers combined and dried over anhydrous magnesium sulfate. The residue was applied onto a silica gel column with methanol:CH2Cl2 (1:30) to yield 4-methoxy-3-methyl-1-phenyl-6-(4-piperazin-1-yl-phenyl)-1H-pyrazolo[3,4-b]pyridine as a white solid.

WORKUP

后处理

  1. customInto a 50 mL round-bottom flask, was placed
  2. concentrationThe resulting mixture was concentrated under vacuum
  3. extractionThe resulting solution was extracted with of ethyl acetate (3×10 mL)
  4. dry with materialdried over anhydrous magnesium sulfate