Methyl iodide → 2,3-Difluoroanisole

To a solution of 2,3-difluorophenol 21a (2.08 g, 14.5 mmol, purchased from Beijing yu xiang hui da chemical Co., Ltd) in acetone (50 mL) were added methyl iodide (1.24 mL, 19.98 mmol) and potassium carbonate (3.18 g, 23.06 mmol) in turn at room temperature. The mixture was stirred at room temperature for 16 hours and then filtered. To the filtrate was added ethyl acetate (40 mL). The resulting mixture was washed with water (40 mL×2), dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo to give the title compound 21b as yellow oil (2.09 g, 100%). This material was not further purified. The compound was characterized by the following spectroscopic data: 1H NMR (400 MHz, CDCl3) δ(ppm): 7.01 (m, 1H), 6.83-6.71 (m, 2H), 3.92 (s, 3H).

1. filtrationfiltered
2. additionTo the filtrate was added ethyl acetate (40 mL)
3. washThe resulting mixture was washed with water (40 mL×2)
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated in vacuo

ORD record

ord-daefb61f4f7543f4b0ee153ab29d54d1

Source dataset

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09394329B2