反应详情

温度

70 °C

Under a stream of nitrogen gas, 0.399 g of 3,3,3-trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone), compound 3-3 was dissolved in 2.4 ml of pyridine at room temperature. To this solution were added 0.133 ml of piperidine and 0.159 g of methylmalonic acid. and the mixture was heated to 70° C. and stirred for 3.5 hours. Then, 2.4 ml of acetic acid was added, and stirring was further continued at 130° C. for 8 hours. The reaction solution was left cooling to room temperature and concentrated under reduced pressure. The residue was diluted with 100 ml of diethyl ether. The diluted solution was washed twice with 20 ml of 3 N hydrochloric acid and once with 30 ml of saturated sodium bicarbonate solution, dried with magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was subjected to column chromatography to give 0.255 g of 2-(2-fluoro-4-chloro-5-isopropoxyphenyl)-4-methyl-5-trifluoromethylpyridazin-3-one, compound 5-2.

1. stirringstirring
2. waitwas further continued at 130° C. for 8 hours
3. waitThe reaction solution was left
4. temperaturecooling to room temperature
5. concentrationconcentrated under reduced pressure
6. additionThe residue was diluted with 100 ml of diethyl ether
7. washThe diluted solution was washed twice with 20 ml of 3 N hydrochloric acid and once with 30 ml of saturated sodium bicarbonate solution
8. dry with materialdried with magnesium sulfate
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure