HRID1249932
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- washwashed with saturated ammonium chloride solution
- customThe organic layer was separated
- extractionthe aqueous layer was extracted with dichloromethane (3×100 ml)
- dry with materialThe combined organic layers were dried over sodium sulphate
- customevaporated
- customA brown solid was obtained
- customa brown solid was obtained