Potassium Carbonate → 1-Chloro-2-(difluoromethoxy)-3-fluorobenzene

Temperature

100 °C

2-Chloro-6-fluorophenol (1.8 g, 12.33 mmol) was dissolved in dimethylformamide (DMF; 22 mL) and water (2.2 mL). Potassium carbonate (2.55 g, 18.5 mmol) and sodium chlorodifluoroacetate (4.7 g, 30.8 mmol) were then added and the solution was heated to 100° C. for 3 h. The cooled reaction mixture was then diluted with concentrated HCl (10 mL) and the resulting solution was stirred for 2 h. The reaction mixture was diluted with diethyl ether, washed with water, washed twice with 1M NaOH, washed once with brine, dried, filtered and concentrated under vacuum to yield the title compound (1 g, 41% yield) that was used in subsequent reactions without further purification.

1. customThe cooled reaction mixture
2. washwashed with water
3. washwashed twice with 1M NaOH
4. washwashed once with brine
5. customdried
6. filtrationfiltered
7. concentrationconcentrated under vacuum

ORD record

ord-0265a73d97804f28b16f58482a289d12

Source dataset

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08658791B2