反应详情

To a mixture of 1.33 g (0.0049 mol) of 4-(2,4-dichlorobenzoyl)-1-methyl-5-hydroxypyrazole, 0.54 g (0.0054 mol) of triethylamine and 30 ml of toluene was added 1.3 g (0.0059 mol) of o-chlorobenzyl methanesulfonate. Then, the reaction mixture was refluxed with stirring for 2 hours. After cooling, the reaction mixture was washed with 20 ml of water three times, and the organic layer was separated. After drying over anhydrous sodium sulfate, the organic layer was concentrated under reduced pressure and was subjected to a column chromatography (silica gel, eluent; ethyl acetate:benzene=1:9) to obtain 1.5 g of the title compound (yield: 77%).

1. temperatureThen, the reaction mixture was refluxed
2. temperatureAfter cooling
3. washthe reaction mixture was washed with 20 ml of water three times
4. customthe organic layer was separated
5. dry with materialAfter drying over anhydrous sodium sulfate
6. concentrationthe organic layer was concentrated under reduced pressure