反应详情

A mixture comprising 1.48 g of 2-i-propyl-4,5-dibromo-3(2H)pyridazinone, 1.68 g of 2-methoxy-1-naphthylmethylamine hydrochloride, 1.33 g of sodium carbonate, 30 ml of water and 30 ml of 1,4-dioxane, was refluxed under stirring overnight. Then, 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 sequentially with a 2 wt% hydrochloric acid aqueous solution, water and a saturated sodium chloride aqueous solution and then dried over sodium sulfate. Then, the solvent was distilled off. The residual solid thus obtained was crystallized from ethyl acetate/n-hexane to obtain 1.18 g of the above identified compound as colorless crystals having a melting point of from 160° to 161° C.

1. temperaturewas refluxed
2. distillationThen, the 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 sequentially with a 2 wt% hydrochloric acid aqueous solution, water
7. dry with materiala saturated sodium chloride aqueous solution and then dried over sodium sulfate
8. distillationThen, the solvent was distilled off
9. customThe residual solid thus obtained
10. customwas crystallized from ethyl acetate/n-hexane
11. customto obtain 1.18 g of the
12. customof from 160° to 161° C.