HRID1277941

反应详情

EQUATION

反应方程式

HRID 1277941 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.55 g of 6-(3,5-dichloro-4-methylphenyl)-3-pyridazone, 1.43 g of butyl chloroformate, 1.75 g of potassium carbonate and 100 ml of acetonitrile was heated under reflux for 7.5 hours. After cooling the reaction mixture, the unreacted pyridazone and inorganic salts were removed by filtration and the solvent was distilled under reduced pressure from the filtrate. The residue was recrystallized from hexane, giving 1.1 g (31%) of the desired Compound No. 32, in the form of needles, whose melting point and spectroscopic data agreed completely with those of the compound obtained in Example 6.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 7.5 hours
  3. temperatureAfter cooling the reaction mixture
  4. customthe unreacted pyridazone and inorganic salts were removed by filtration
  5. distillationthe solvent was distilled under reduced pressure from the filtrate
  6. customThe residue was recrystallized from hexane