HRID2267909

反应详情

EQUATION

反应方程式

HRID 2267909 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

4-(2-Methyl-thiazol-4-ylmethoxy)-indole-1,2-dicarboxylic acid 1-tert-butyl ester 2-ethyl ester (169) (1.75 g, 4.2 mmol) is dissolved in 20 ml of ethanol. After addition of a 0.5M aqueous sodium hydroxide solution (33.6 ml, 16.8 mmol) the solution is heated to 60° C. and stirred at this temperature for 18 h. Then the reaction mixture is evaporated and the residue is dissolved in ethyl acetate. AT 0° C. conc HCl is added until a pH of 1 is reached. The organic phase is washed with water and brine. The organic layers are dried over sodium sulphate, filtrated. The product crystallized upon evaporation and could be filtrated off.

WORKUP

后处理

  1. customThen the reaction mixture is evaporated
  2. dissolutionthe residue is dissolved in ethyl acetate
  3. additionAT 0° C. conc HCl is added until a pH of 1
  4. washThe organic phase is washed with water and brine
  5. dry with materialThe organic layers are dried over sodium sulphate
  6. filtrationfiltrated
  7. customThe product crystallized upon evaporation
  8. filtrationcould be filtrated off