HRID559144

反应详情

EQUATION

反应方程式

HRID 559144 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

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

WORKUP

后处理

  1. concentrationThe reaction mixture is concentrated under vacuum
  2. extractionthe product is extracted with EtOAc
  3. washthe organic phase is washed with a saturated NaCl solution
  4. dry with materialdried over MgSO4
  5. customthe solvent is evaporated off under vacuum
  6. customThe residue is triturated in a PE/EtOAc (90/10; v/v) mixture
  7. customthe precipitate formed
  8. customis filter-dried