HRID1031525

反应详情

EQUATION

反应方程式

HRID 1031525 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl-2-(2-methylbenzyliden)acetoacetate (0.050 mol) is added to 1-methyl-3-phenyl-5-pyrazolamine (0.050 mol) in ethanol (50 ml) and refluxed for 90 minutes. The mixture is then cooled to room temperature, further ethyl-2-(2-methylbenzyliden)acetoacetate (0.050 mol) is added thereto, and the mixture refluxed for further 90 minutes. The reaction mixture is then cooled, the solvent is evaporated, and the residue is taken up in ethyl ether, collected by filtration, and dried. The product is dissolved in methanol and a mixture of hydrochloric acid and methanol (45 mmol of HCl) is added thereto. The product of the title precipitates by adding ethyl ether. M.p. 187° C. (dec.).

WORKUP

后处理

  1. temperaturerefluxed for 90 minutes
  2. temperaturethe mixture refluxed for further 90 minutes
  3. temperatureThe reaction mixture is then cooled
  4. customthe solvent is evaporated
  5. filtrationcollected by filtration
  6. customdried
  7. dissolutionThe product is dissolved in methanol
  8. additionis added
  9. customThe product of the title precipitates
  10. additionby adding ethyl ether