Ethyl Bromide → 1-Bromo-4-ethoxy-2,3-difluorobenzene

Temperature

80 °C

Sodium hydroxide (75.9 g) was added to a water (400 ml) solution of 4-bromo-2,3-difluorophenol (T-1) (195.0 g), bromoethane (196.2 g) and tetrabutylammonium bromide (hereinafter abbreviated as TBAB) (24.2 g), and the mixture was heated at 80° C. for 6 hours with stirring under an atmosphere of nitrogen. After the reaction had been completed, the reaction mixture was extracted with heptane and the organic layer was washed successively with water and brine, and dried over anhydrous magnesium sulfate. The extract was concentrated under reduced pressure to give a black oil. The oil was purified by distillation to give 1-ethoxy-2,3-difluorobromobenzene (T-2) (230.0 g, 97% yield) as a colorless oil.

1. extractionthe reaction mixture was extracted with heptane
2. washthe organic layer was washed successively with water and brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationThe extract was concentrated under reduced pressure
5. customto give a black oil
6. distillationThe oil was purified by distillation

ORD record

ord-22eb131bb11441c79083344e243369f7

Source dataset

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08304037B2