HRID1278228

反应详情

EQUATION

反应方程式

HRID 1278228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3.50 g. of 3-dimethylamino-1-(3-pyridyl)-2-propen-1-one, 25 L ml. of glacial acetic acid and 2.44 g. of 3-amino-5-methylpyrazole-4-carbonitrile is refluxed 6 hours. The solvent is removed in vacuo. The residue is dissolved in dichloromethane and the solution washed with saturated sodium bicarbonate solution. The dichloromethane layer is dried over anhydrous sodium sulfate and pased through a column of hydrous magnesium silicate. The eluent is concentrated and hexane added to give 2.60 g. of the product of the example, m.p. 245°-246° C.

WORKUP

后处理

  1. additionA mixture of 3.50 g
  2. customThe solvent is removed in vacuo
  3. dissolutionThe residue is dissolved in dichloromethane
  4. washthe solution washed with saturated sodium bicarbonate solution
  5. dry with materialThe dichloromethane layer is dried over anhydrous sodium sulfate
  6. concentrationThe eluent is concentrated
  7. additionhexane added
  8. customto give 2.60 g