反应详情

温度

80 °C

First, 0.25 g of 3,3,3-trifluoro-2-oxopropanal 1-(4-chlorophenylhydrazone), compound 3-11 was dissolved in 2 ml of pyridine. To this solution were added 0.24 g of methylmalonic acid and 0.09 g of piperidine, and the mixture was stirred at 80° C. for 4 hours. Then, 2.0 ml of acetic acid was added, and the mixture was stirred at 80° C. for 6.5 hours and further at 120° C. for 4 hours. After completion of the reaction, the reaction solution was poured into water, and this mixture was extracted with diethyl ether. The organic layer was washed with water and then with diluted hydrochloric acid, dried with anhydrous magnesium sulfate, and evaporated to remove the diethyl ether. The residue was subjected to silica gel column chromatography to give 0.15 g of 2-(4-chlorophenyl)-4-methyl-5-trifluoromethylpyridazin-3-one, compound 5-12, m.p., 80.8° C.

1. stirringthe mixture was stirred at 80° C. for 6.5 hours and further at 120° C. for 4 hours
2. customAfter completion of the reaction
3. extractionthis mixture was extracted with diethyl ether
4. washThe organic layer was washed with water
5. dry with materialwith diluted hydrochloric acid, dried with anhydrous magnesium sulfate
6. customevaporated
7. customto remove the diethyl ether