反应详情

1.27 g of 6-(3,5-dichloro-4-methylphenyl)-3-pyridazone and 1.12 L g of triethylenediamine were suspended in 25 ml of acetonitrile, and then 1.5 g of morpholinocarbonyl chloride were added dropwise thereto. When the addition was complete, the mixture was stirred at room temperature for 30 minutes and then the white precipitate thus produced was removed by filtration. The filtrate was concentrated by evaporation under reduced pressure and then extracted with chloroform. The solvent was distilled under reduced pressure from the extract, giving a crude product which, after recrystallization from a mixture of benzene and hexene, gave 1.72 g (94%) of the desired Compound No. 10, melting at 155°-159° C.

1. additionWhen the addition
2. customthe white precipitate thus produced
3. customwas removed by filtration
4. concentrationThe filtrate was concentrated by evaporation under reduced pressure
5. extractionextracted with chloroform
6. distillationThe solvent was distilled under reduced pressure from the extract
7. customgiving a crude product which
8. customafter recrystallization
9. additionfrom a mixture of benzene and hexene