反应详情

13 g of 4-bromo-1-(2,4,6-trichlorophenyl)-3-(3-octadecylureido)-2-pyrazolin-5-one and 10 g of 3-methyl-4-nitropyrazole were mixed at 90° C. for 2 hours. To the reaction mixture, 200 ml of ethyl acetate was added and the mixture was washed several times with water. The ethyl acetate layer was dried with anhydrous sodium sulfate and concentrated. The residual oil was dissolved in 50 ml of chloroform and purified with column chromatography using 500 g of silica gel (art 7734 manufactured by MERCK & Co.) wetted with chloroform as a bulking agent. Upon elution with a solvent mixture of chloroform and ethyl acetate (10:1), 10.9 g of an oily comprising the desired coupler was obtained.

1. washthe mixture was washed several times with water
2. dry with materialThe ethyl acetate layer was dried with anhydrous sodium sulfate
3. concentrationconcentrated
4. dissolutionThe residual oil was dissolved in 50 ml of chloroform
5. custompurified with column chromatography
6. washUpon elution
7. additionwith a solvent mixture of chloroform and ethyl acetate (10:1), 10.9 g of an oily comprising the desired coupler
8. customwas obtained