Hydrochloric Acid → 1-(2,4-Difluorophenyl)-2-methylpropan-1-one

To a mixture of 120 g (0.68 mmol) of 2,4-difluorobenzoyl chloride, 3.7 g (37 mmol) of copper (I) chloride, and 400 ml of diethyl ether was added dropwise 442 ml of diethyl ether containing 130.2 g (0.88 mol) of isopropylmagnesium bromide at -25° C. over 4 hours. The temperature was elevated up to -5° C., and the mixture was stirred at that temperature for 30 minutes. To the reaction mixture were added dropwise 150 ml of water and then 120 ml of 6N hydrochloric acid. The organic layer was separated, washed successively with 5% hydrochloric acid, a saturated sodium chloride aqueous solution, a saturated sodium carbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried. The solvent was removed by distillation under reduced pressure, and the residue was distilled under reduced pressure to obtain 104.3 g (83%) of 1-(2,4-difluorophenyl)-2-methylpropan-1-one as a colorless oily substance.

1. customwas elevated up to -5° C.
2. customThe organic layer was separated
3. washwashed successively with 5% hydrochloric acid
4. dry with materiala saturated sodium chloride aqueous solution, a saturated sodium carbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried
5. customThe solvent was removed by distillation under reduced pressure
6. distillationthe residue was distilled under reduced pressure

ORD record

ord-51558a2503c74c99963c45f2e6327c40

Source dataset

uspto-grants-1994_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05312815