Hydrochloric Acid → 3-[3-(6-Hydroxy-m-tolyl)-1,2-benzisoxazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione

온도

-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.

ORD 기록

ord-9eedda6a491d4e08a95c44028e909775

출처 데이터셋

uspto-grants-2000_12

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06156700