Bromine → 1,2-Benzenediol, 4-bromo-3-fluoro- (9CI)

온도

-10 °C

3-Fluorocatechol (7.2 g) in 50 ml of carbon tetrachloride and 40 ml of chloroform are treated at -10° C. within 10 minutes with a solution of 2.88 ml of bromine in 30 ml of carbon tetrachloride. After stirring at -10° C. for 1 hour the reaction mixture is filtered. The residual solid is washed with a small amount of cold carbon tetrachloride and dried. There are obtained 6.30 g of 4-bromo-3-fluorocatechol as a white powder. This is treated with 6.0 ml of diphenylchloromethane and heated to 130° C. within 1 hour. Subsequently, the product is distilled at 135° C./0.05 Torr and recrystallized from ethanol. There are obtained 6.40 g of 5-bromo-4-fluoro-2,2-diphenyl-1,3-benzodioxol as a white crystalline powder of m.p. 61.5°-63° C.

1. filtrationis filtered
2. washThe residual solid is washed with a small amount of cold carbon tetrachloride
3. customdried

ORD 기록

ord-87a04f41b5644a77b8d8dfbfc2297062

출처 데이터셋

uspto-grants-1995_08

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US05438052