Hydrochloric Acid → (E)-2-(3-Chloroprop-1-en-1-yl)-1,4-difluorobenzene

Temperature

100 °C

A mixture of (2E)-3-(2,5-difluorophenyl)prop-2-en-1-ol (Intermediate 70, 700 mg, 4.12 mmol), 1,4-dioxane (5 mL), and hydrochloric acid (12.1 M, 1 mL) was heated in the microwave at 100° C. for 3 hours. It was concentrated to dryness under reduced pressure, the residue taken up in ethyl acetate (10 mL), washed with water (1×10 mL), saturated sodium bicarbonate solution, brine and dried over sodium sulfate. The solvent was removed under reduced pressure to give 688 mg (89% yield) of product as a yellow oil.

1. concentrationIt was concentrated to dryness under reduced pressure
2. washwashed with water (1×10 mL), saturated sodium bicarbonate solution, brine
3. dry with materialdried over sodium sulfate
4. customThe solvent was removed under reduced pressure

ORD record

ord-7cb5c0a2c39945ed9583768b7eadd637

Source dataset

uspto-grants-2011_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07875715B2