1-(4-Fluorophenyl)ethanol → 1-(1-Bromoethyl)-4-fluorobenzene

0.5 g of 1-(4-fluorophenyl)ethanol is dissolved in 20 cm3 of dichloromethane, under an inert atmosphere, at a temperature close to 20° C. 1.24 cm3 of pure bromo(trimethyl)silane are introduced in two lots to the reaction mixture. The latter is stirred at a temperature close to 20° C. for 48 h, then it is washed with a saturated aqueous solution of sodium chloride, dried over a phase separation cartridge and concentrated using a rotary evaporator under reduced pressure (5 kPa). The 700 mg of crude product obtained are purified by filtration through a silica pellet (eluent: 10% ethyl acetate/90% cyclohexane). After concentrating the fractions under reduced pressure, 439 mg of 1-(1-bromoethyl)-4-fluorobenzene are obtained in the form of a colorless thick oil.

1. customclose to 20° C
2. customclose to 20° C. for 48 h
3. washit is washed with a saturated aqueous solution of sodium chloride
4. customdried over a phase separation cartridge
5. concentrationconcentrated
6. customa rotary evaporator under reduced pressure (5 kPa)

ORDレコード

ord-45567561ff1c4ecf9cfba6aac71202f4

出典データセット

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08372864B2