HRID1269926

反应详情

EQUATION

反应方程式

HRID 1269926 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trifluoroacetic acid (1 ml) was added to a solution of 4-(methylthio)-1-tetrahydro-2H-pyran-2-yl-5-(tetrahydro-2H-pyran-2-yloxy)-1H-indazole (0.0730 g, 0.21 mmol) in dichloromethane (1 ml) and stirred for 1 hour. The reaction solution was added to water and extracted three times with ethyl acetate and the extract solution was dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by a silica gel chromatography (hexane/ethyl acetate=2/1), crystallized from hexane/ethyl acetate and then dried up to obtain 4-(methylthio)-1H-indazol-5-ol (0.0481 g, >99%).

WORKUP

后处理

  1. extractionextracted three times with ethyl acetate
  2. dry with materialthe extract solution was dried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off
  4. customthe residue was purified by a silica gel chromatography (hexane/ethyl acetate=2/1)
  5. customcrystallized from hexane/ethyl acetate
  6. customdried up