反应详情

温度

160 °C

A flask equipped with a claisen distillation head and magnetic stirring was charged with an intimate mixture of 32.6 g (0.097 mole) 1-[(4-chlorophenyl)thio]-1-[(4-methoxyphenyl) hydrazono]-2-propanone, 24.8 ml of ethylcyanoacetate and 12.2 g of ammonium acetate. The mixture was heated under a nitrogen atmosphere at 160° C. for 30 min. The reaction mixture was cooled and dissolved in methylene chloride. The organic layer was washed successively with saturated aqueous sodium bicarbonate and water. The organic layer was dried over magnesium sulfate and evaporated in vacuao to yield semi pure product. The residue was recrystallized from 1900 ml of ethanol to yield 6-[(4-chlorophenyl)thio]-2,3-dihydro-2-(4-methoxyphenyl)-5-methyl-3-oxo-4-pyridazinecarbonitrile, mp 146-148° C. (EtOH).

1. customA flask equipped with a claisen distillation head
2. temperatureThe reaction mixture was cooled
3. washThe organic layer was washed successively with saturated aqueous sodium bicarbonate and water
4. dry with materialThe organic layer was dried over magnesium sulfate
5. customevaporated in vacuao
6. customto yield semi pure product
7. customThe residue was recrystallized from 1900 ml of ethanol