HRID1749866

反应详情

EQUATION

反应方程式

HRID 1749866 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

A solution of methyl 5-chloro-1H-indazole-3-carboxylate (2.11 g, 10.0 mmol) in THF (70 mL) was cooled to −10° C., and added dropwise with a 1 M solution of diisobutylaluminum hydride in toluene (36.0 mL). After completion of the addition, the mixture was stirred at −10° C. for 1 hour, and then stirred overnight at room temperature. The reaction mixture was added dropwise with saturated aqueous sodium sulfate under ice cooling to terminate the reaction, and then the reaction mixture was filtered through Celite. The filtrate was concentrated, and the resulting residue was purified by silica gel column chromatography (chloroform/methanol) to obtain the objective (5-chloro-1H-indazol-3-yl)methanol (0.210 g, 11%).

WORKUP

后处理

  1. additionAfter completion of the addition
  2. stirringstirred overnight at room temperature
  3. customto terminate
  4. customthe reaction
  5. filtrationthe reaction mixture was filtered through Celite
  6. concentrationThe filtrate was concentrated
  7. customthe resulting residue was purified by silica gel column chromatography (chloroform/methanol)