HRID1794588

反应详情

EQUATION

反应方程式

HRID 1794588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

N-(5-Bromo-4-methyl-2-propylimidazol-1-yl)-2-ethoxybenzamide from Example 2a (0.5 g, 1.2 mmol) and copper(I) cyanide (0.3 g, 3.5 mmol) are introduced into 12.5 ml of pyridine and heated at 100° C. for 6 hours. Potassium iodide (23 mg, 0.56 mmol) is added to the mixture, which is then stirred for a further 6 hours at 100° C. The reaction mixture is cooled to room temperature and, after addition of 50 ml of ethyl acetate, washed with dilute alkaline H2O2 solution. The aqueous phase is re-extracted with ethyl acetate, and the combined ethyl acetate phase is concentrated, finally azeotroped with toluene and again concentrated.

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled to room temperature
  2. washwashed
  3. additionwith dilute alkaline H2O2 solution
  4. extractionThe aqueous phase is re-extracted with ethyl acetate
  5. concentrationthe combined ethyl acetate phase is concentrated
  6. customfinally azeotroped with toluene
  7. concentrationagain concentrated