HRID1749864

反应详情

EQUATION

反应方程式

HRID 1749864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

A solution of methyl 5-fluoro-1H-indazole-3-carboxylate (0.582 g, 3.00 mmol) in THF (20 mL) was cooled to −10° C., and added dropwise with a 1 M solution of diisobutylaluminum hydride in toluene (10.8 mL, 10.8 mmol) over 5 minutes. The reaction mixture was stirred at −10° C. for 1 hour, and then overnight at room temperature. The reaction mixture was added dropwise with saturated aqueous sodium sulfate under ice cooling to terminate the reaction, and then filtered through Celite. The filtrate was concentrated, and the resulting residue was purified by silica gel column chromatography (chloroform/methanol) to obtain (5-fluoro-1H-indazol-3-yl)methanol (0.217 g, 43%).

WORKUP

后处理

  1. customovernight
  2. customat room temperature
  3. customto terminate
  4. customthe reaction
  5. filtrationfiltered through Celite
  6. concentrationThe filtrate was concentrated
  7. customthe resulting residue was purified by silica gel column chromatography (chloroform/methanol)