HRID727844

反应详情

EQUATION

反应方程式

HRID 727844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

4.9 g of the amide of example 3 is dissolved in 50 ml of dioxane and 3.23 ml of pyridine and mixed with 3.16 ml of trifluoroacetic acid anhydride under ice cooled at 5° C. internal temperature. After 20 hours of stirring at room temperature it is added to half-saturated potassium carbonate solution, extracted with ether and the ether phase is dried and concentrated by evaporation. After distillation on a bulb tube at 200°-215° C./0.05 mbar, 3.2 g of 4-[1-(1-imidazolyl)-butyl]-benzonitrile is obtained, which, after crystallization from ether, melts at 63°-71° C.

WORKUP

后处理

  1. extractionextracted with ether
  2. dry with materialthe ether phase is dried
  3. concentrationconcentrated by evaporation
  4. distillationAfter distillation on a bulb tube at 200°-215° C./0.05 mbar