HRID1278229

反应详情

EQUATION

反应方程式

HRID 1278229 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.90 g. of 3-dimethylamino-2-methyl-1-(3-pyridyl)-2-propen-1-one and 1.22 g. of 3-amino-5-methylpyrazole-4-carbonitrile in 25 ml. of glacial acetic acid is refluxed for 6 hours. The solvent is removed in vacuo and the residue partitioned between dichloromethane and saturated sodium bicarbonate solution. The dichloromethane layer is separated, dried over anhydrous sodium sulfate and passed through a column of hydrous magnesium silicate. The eluent is concentrated and hexane added to give 0.95 g. of the product of the example, m.p. 207°-209° C.

WORKUP

后处理

  1. additionA mixture of 1.90 g
  2. customThe solvent is removed in vacuo
  3. customthe residue partitioned between dichloromethane and saturated sodium bicarbonate solution
  4. customThe dichloromethane layer is separated
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationThe eluent is concentrated
  7. additionhexane added
  8. customto give 0.95 g