HRID55358

反应详情

EQUATION

反应方程式

HRID 55358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.50 g of 1-(4-methylphenyl)-5-(4-chlorophenyl)pyrazole-3-carboxylic acid chloride in ml of CH2Cl2 is added dropwise to 100 ml of a 33% solution of methylamine in ethanol. After stirring for hours at room temperature, the mixture is concentrated under vacuum, the residue is taken up with a mixture of 5% Na2CO3 +AcOEt, the organic phase is decanted, washed with a saturated solution of NaCl and dried over MgSO4 and the solvents are evaporated off. The residue is taken up in isopropyl ether and the crystals obtained are filtered off and dried under vacuum to give 0.44 g of the expected amide.

WORKUP

后处理

  1. concentrationthe mixture is concentrated under vacuum
  2. additionthe residue is taken up with a mixture of 5% Na2CO3 +AcOEt
  3. customthe organic phase is decanted
  4. washwashed with a saturated solution of NaCl
  5. dry with materialdried over MgSO4
  6. customthe solvents are evaporated off
  7. customthe crystals obtained
  8. filtrationare filtered off
  9. customdried under vacuum