HRID1277941
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureunder reflux for 7.5 hours
- temperatureAfter cooling the reaction mixture
- customthe unreacted pyridazone and inorganic salts were removed by filtration
- distillationthe solvent was distilled under reduced pressure from the filtrate
- customThe residue was recrystallized from hexane