反应详情

2.85 g of 4-(2,4-dichlorobenzoyl)-1,3-dimethyl-5-hydroxypyrazole was dissolved in 50 ml of acetonitrile, and 1.38 g of potassium carbonate (anydrous) was added thereto. The resultant mixture was stirred at room temperature for 2 hours, 2.14 g of β-bromoethyl-N-methylaniline was added, and the mixture heated for 3 hours under reflux. After cooling, crystals were filtered off. The filtrate was distilled under reduced pressure and the residue was purified by silica gel chromatography (eluent, benzene:ethyl acetate at 8:1) to give 3.82 g of the desired product, Compound 2, having nD24 1.5975 (yield 91.4%).

1. temperaturethe mixture heated for 3 hours
2. temperatureunder reflux
3. temperatureAfter cooling
4. filtrationcrystals were filtered off
5. distillationThe filtrate was distilled under reduced pressure
6. customthe residue was purified by silica gel chromatography (eluent, benzene:ethyl acetate at 8:1)