反应详情

A mixture comprising 564 mg of 2-ethyl-4,5-dibromo-3(2H)pyridazinone, 291 mg of 2-furanylmethylamine, 530 mg of sodium carbonate, 15 ml of water and 15 ml of 1,4-dioxane, was refluxed under stirring for 5 hours. The solvent was distilled off under reduced pressure, and water was poured to the residue thus obtained. The mixture was extracted with ethyl acetate. The extract was washed with water and dried over sodium sulfate. Then, the solvent was distilled off. The residue oily substance thus obtained was purified by silica gel column chromatography by using a mixture of benzene/ethyl acetate (volume ratio of 2/1) as developer to obtain 294 mg of the above identified compound as colorless crystals having a melting point of from 120° to 123° C. (as recrystallized from a mixture of ethyl acetate/ethyl ether/n-hexane).

1. temperaturewas refluxed
2. distillationThe solvent was distilled off under reduced pressure, and water
3. additionwas poured to the residue
4. customthus obtained
5. extractionThe mixture was extracted with ethyl acetate
6. washThe extract was washed with water
7. dry with materialdried over sodium sulfate
8. distillationThen, the solvent was distilled off
9. customThe residue oily substance thus obtained
10. customwas purified by silica gel column chromatography
11. additiona mixture of benzene/ethyl acetate (volume ratio of 2/1) as developer
12. customto obtain 294 mg of the
13. customof from 120° to 123° C.
14. customas recrystallized from a mixture of ethyl acetate/ethyl ether/n-hexane)