HRID1165178

反应详情

EQUATION

反应方程式

HRID 1165178 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl-1-methylindole-carboxylate* (6.0 g) in trifluoroacetic acid (50 ml) is cooled in an ice bath as sodium borohydride pellets (6.0 g) are added slowly, keeping the temperature below 10° C. The slurry is allowed to rise to room temperature and then stirred overnight. The unreacted sodium borohydride is decomposed with 50% sodium hydroxide and the mixture is extracted several times with ether. The extracts are washed with saturated sodium chloride solution, dried over sodium sulfate, and evaporated to dryness to obtain an orange oil. This is distilled in a kuegelrohr (b.p.=128-150/0.2 mm) to yield colorless liquid, methyl-2, 3-dihydro-1-methylindole-carboxylate.

WORKUP

后处理

  1. additionare added slowly
  2. customthe temperature below 10° C
  3. customto rise to room temperature
  4. extractionthe mixture is extracted several times with ether
  5. washThe extracts are washed with saturated sodium chloride solution
  6. dry with materialdried over sodium sulfate
  7. customevaporated to dryness
  8. customto obtain an orange oil
  9. distillationThis is distilled in a kuegelrohr (b.p.=128-150/0.2 mm)