HRID2053231

反应详情

EQUATION

反应方程式

HRID 2053231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

1-Methyl-5-nitro-1H-indole-2-carboxylic acid methyl ester (70 mg, 0.3 mmol) was dissolved in DMF (5 ml) and SnCl2.2H2O (339 mg, 1.5 mmol) was added as a solid. The resulting solution was stirred at 60° C. for 4 h. After cooling to room temperature, a pre-mixed aqueous solution of saturated Rochelle's salt (3 ml) and saturated NaHCO3 (3 ml) was added to the reaction mixture and the aqueous layer was extracted with EtOAc (3×6 ml). The organic layer was washed with H2O (3 ml), 1:1 NaHCO3:Rochelle's salt solution (3 ml), dried (MgSO4), filtered and the solvent was removed in vacuo to give the title compound.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. extractionthe aqueous layer was extracted with EtOAc (3×6 ml)
  3. washThe organic layer was washed with H2O (3 ml), 1:1 NaHCO3
  4. dry with materialRochelle's salt solution (3 ml), dried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent was removed in vacuo