反应详情

Separately 0.38 g of 1-ethyl-5-hydroxypyrazole hydrochloride was dissolved in 10 ml of chloroform, and 0.52 g of triethylamine was added, while cooling with ice. Into the obtained solution was added dropwise 5 ml of a chloroform solution containing the previously obtained 3-(isoxazol-3-yl)-4-methylsulfonyl-2-methylbenzoyl chloride to stir at room temperature for an hour. To the reaction mixture were added 0.26 g of triethylamine and 0.05 g of acetone cyanohydrin to further stir overnight. The reaction solution was washed with dilute hydrochloric acid, with water, then with a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was distilled out under reduced pressure. Methanol was added to the obtained residue. The produced crystals were separated by filtration to give 0.18 g of the title compound as white crystals. m.p. 85~88° C.

1. temperaturewhile cooling with ice
2. washThe reaction solution was washed with dilute hydrochloric acid, with water
3. dry with materialwith a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate
4. distillationThe solvent was distilled out under reduced pressure
5. additionMethanol was added to the obtained residue
6. customThe produced crystals were separated by filtration