HRID1242125

反应详情

EQUATION

反应方程式

HRID 1242125 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a mixed solvent of tetrahydrofuran (30 ml), ethanol (30 ml) and water (100 ml), added are methyl E-4-(2-dimethylaminovinyl)-3-nitrobenzoate (10.0 g) and sodium hydrosulfite (104.5 g), and stirred at 70° C. for 1 hours. After this is cooled to room temperature, a saturated saline solution is added thereto. Then, this is extracted with chloroform. The organic layer is dried, and the solvent is evaporated away. The resulting residue is purified through silica gel column chromatography (eluent: hexane/ethyl acetate=2/1 to 1/1) to obtain 6-methoxycarbonylindole (2.79 g).

WORKUP

后处理

  1. temperatureAfter this is cooled to room temperature
  2. additiona saturated saline solution is added
  3. extractionThen, this is extracted with chloroform
  4. customThe organic layer is dried
  5. customthe solvent is evaporated away
  6. customThe resulting residue is purified through silica gel column chromatography (eluent: hexane/ethyl acetate=2/1 to 1/1)