HRID1159641

反应详情

EQUATION

反应方程式

HRID 1159641 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of 5 g of 4-cyanophenylhydrazine hydrochloride in 40 ml of acetic acid is admixed with 2.7 g of sodium acetate and then heated at 80° C. for 20 hours. The reaction mixture is concentrated under vacuum, the residue is taken up in water and extracted with AcOEt, the organic phase is washed with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated under vacuum. The residue is triturated in a PE/AcOEt mixture (90/10; v/v) and the precipitate formed is filtered off with suction. This gives 4.8 g of the expected compound.

WORKUP

后处理

  1. concentrationThe reaction mixture is concentrated under vacuum
  2. extractionextracted with AcOEt
  3. washthe organic phase is washed with saturated NaCl solution
  4. dry with materialdried over MgSO4
  5. customthe solvent is evaporated under vacuum
  6. customThe residue is triturated in a PE/AcOEt mixture (90/10; v/v)
  7. customthe precipitate formed
  8. filtrationis filtered off with suction