反应详情

温度

-10 °C

A mixture of 3-[3-(6-methoxy-m-tolyl)-1,2-benzisoxazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione (5.00 g, 0.0116 mol) in methylene chloride is cooled to -10° C., treated dropwise with 15.1 mL of 1 M boron tribromide in methylene chloride while maintaining the reaction mixture temperature at -15° C. to 0° C., warmed to room temperature, treated dropwise with 5 mL of the boron tribromide solution, stirred at room temperature for one hour, and poured into dilute hydrochloric acid. The resultant aqueous mixture is diluted with acetone, concentrated In vacuo, diluted with water, and filtered to obtain a solid. The solid is washed with water and dried in a vacuum oven at 60° C. to give the title product as a yellow solid which is identified by mass spectral analysis.

1. temperaturewhile maintaining the reaction mixture temperature at -15° C. to 0° C.
2. temperaturewarmed to room temperature
3. concentrationconcentrated In vacuo
4. additiondiluted with water
5. filtrationfiltered
6. customto obtain a solid
7. washThe solid is washed with water
8. customdried in a vacuum oven at 60° C.