HRID2181195

反应详情

EQUATION

反应方程式

HRID 2181195 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.37 g (19.0 mmol) of 5-bromo-4-methyl-1H-indole-2-carboxylic acid ethyl ester were dissolved in 150 ml of dioxane; then, 38.1 ml (38.1 mmol) of a lithium hydroxide solution (1 molar in water) were added and the reaction mixture was stirred for 60 hours at room temperature. After evaporation of the solvents, the residue was dissolved in dichloromethane; water was added and the pH adjusted to pH 2-3; then, the mixture was extracted 3 times with dichloromethane. The combined organic phases were washed with water, dried over magnesium sulfate and evaporated to give 4.82 g of crude 5-bromo-4-methyl-1H-indole-2-carboxylic acid as off-white solid.

WORKUP

后处理

  1. customAfter evaporation of the solvents
  2. dissolutionthe residue was dissolved in dichloromethane
  3. additionwater was added
  4. extractionthen, the mixture was extracted 3 times with dichloromethane
  5. washThe combined organic phases were washed with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated