Diethyl Ether → 2,6-Difluoroanisole

In 254 ml of N,N-dimethylformamide was dissolved 25.4 g of 2,6-difluorophenol, followed by adding thereto 29.7 g of potassium carbonate and 83.1 g of iodomethane, and the resulting mixture was stirred at 50° C. for 2 hours. The reaction mixture was added to a mixed solvent of 200 ml of diethyl ether and 600 ml of water and the organic layer was separated. The organic layer obtained was washed with water and then a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then distilled under reduced pressure to remove the solvent. The resulting residue was purified by vacuum distillation (43-45° C./20 mmHg) to obtain 22.9 g of 2,6-difluoroanisole as a colorless oil.

1. additionby adding
2. customthe organic layer was separated
3. customThe organic layer obtained
4. washwas washed with water
5. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
6. distillationdistilled under reduced pressure
7. customto remove the solvent
8. distillationThe resulting residue was purified by vacuum distillation (43-45° C./20 mmHg)

ORD record

ord-c33f70eca4a0418e917994e853fff4dd

Source dataset

uspto-grants-2000_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06025370