HRID1403492

反应详情

EQUATION

反应方程式

HRID 1403492 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-bromo-1H-indole-3-carbaldehyde (5.0 g, 22.3 mmol) in THF (80 mL) was added LiAlH4 (1.70 g, 44.6 mmol). The resulting solution was stirred for 2 h under reflux, then poured into 1N NaOH solution (150 mL), extracted with ethyl acetate (3×100 mL), dried over anhydrous sodium sulfate, and then concentrated under vacuum to give a residue, which was purified via silica gel chromatography (3% ethyl acetate in petroleum ether) to afford 5-bromo-3-methyl-1H-indole as a white solid (3.4 g, 73%).

WORKUP

后处理

  1. temperatureunder reflux
  2. extractionextracted with ethyl acetate (3×100 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under vacuum
  5. customto give a residue, which
  6. customwas purified via silica gel chromatography (3% ethyl acetate in petroleum ether)