反应详情

A mixture comprising 455 mg of 2-ethyl-4,5,6-trichloro-3(2H)pyridazinone, 1.20 g of 3-n-propoxy-4-methoxybenzylamine and 20 ml of ethanol, was refluxed under stirring for 3.5 hours. Ethanol was distilled off under reduced pressure, and water was poured into the residue thereby obtained. The mixture was extracted with ethyl acetate. The extract was washed with dilute hydrochloric acid and water in this order and dried over sodium sulfate. Then, the solvent was distilled off to obtain a light brown viscous oily substance. The product was purified by silica gel column chromatography by using a solvent mixture of benzene-ethyl acetate (15:1 v/v) as the eluent, to obtain 277 mg of the above identified compound. The physical properties and the spectrum data of NMR and MS of the compound completely agreed to those of the compound prepared by the method (1).

1. temperaturewas refluxed
2. distillationEthanol was distilled off under reduced pressure, and water
3. additionwas poured into the residue
4. customthereby obtained
5. extractionThe mixture was extracted with ethyl acetate
6. washThe extract was washed with dilute hydrochloric acid and water in this order
7. dry with materialdried over sodium sulfate
8. distillationThen, the solvent was distilled off
9. customto obtain a light brown viscous oily substance
10. customThe product was purified by silica gel column chromatography
11. additiona solvent mixture of benzene-ethyl acetate (15:1 v/v) as the eluent
12. customto obtain 277 mg of the
13. customprepared by the method (1)