HRID22558

反应详情

EQUATION

反应方程式

HRID 22558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2.13 g of 5-(p-aminophenyl)-5,6,7,8-tetrahydroimidazo[1,5-a]pyridine in 4 ml of concentrated hydrochloric acid and 10 ml of water is cooled in an ice-bath and a solution of 0.78 g of sodium nitrite in 2 ml of water is added slowly. The solution is added via dropping funnel to an ice cooled solution of 3.0 g of copper(I) cyanide in 10 ml of water, keeping the temperature between 30°-40°. The reaction mixture is heated on a steam bath for 1 h, cooled and brought to pH 9. The organic extracts are dried over sodium sulfate and evaporated and the residue is chromatographed on silica gel with ethyl acetate to yield the title compound.

WORKUP

后处理

  1. additionThe solution is added
  2. custombetween 30°-40°
  3. temperatureThe reaction mixture is heated on a steam bath for 1 h
  4. temperaturecooled
  5. dry with materialThe organic extracts are dried over sodium sulfate
  6. customevaporated
  7. customthe residue is chromatographed on silica gel with ethyl acetate