HRID1249932

反应详情

EQUATION

反应方程式

HRID 1249932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
7.5 °C

PROCEDURE

实验过程

5-Methoxyindole-2-carboxylic acid ethyl ester (2 g, 9.13 mmol) and magnesium turnings (0.432 g, 18 mmol) were suspended in dried methanol (30 ml). This mixture was stirred at 5 to 10° C. under nitrogen for 3 hours, then poured into dichloromethane (200 ml), and washed with saturated ammonium chloride solution. The organic layer was separated, and the aqueous layer was extracted with dichloromethane (3×100 ml). The combined organic layers were dried over sodium sulphate and evaporated. A brown solid was obtained. After column chromatography on silica gel using dichloromethane as eluent, a brown solid was obtained.

WORKUP

后处理

  1. washwashed with saturated ammonium chloride solution
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with dichloromethane (3×100 ml)
  4. dry with materialThe combined organic layers were dried over sodium sulphate
  5. customevaporated
  6. customA brown solid was obtained
  7. customa brown solid was obtained