Chlorosulfonic acid → BUTTPARK 120\07-29

A solution of 1-methoxy-2-(trifluoromethyl)benzene (10.0 g, 56.8 mmol) in dry chloroform (76 mL) was cooled to 0° C. and treated with chlorosulfonic acid (7.55 mL, 113.5 mmol) drop-wise under argon. After the addition was completed, the reaction mixture was gradually warmed to room temperature and stirred overnight. The reaction was quenched by pouring the mixture slowly onto ice. The separated, aqueous phase was extracted with chloroform (3×). The combined organic phase was washed sequentially with a saturated, aqueous sodium chloride solution (2×) and water. The organic phase was dried over anhydrous magnesium sulfate and concentrated in vacuo to yield the title compound (8.77 g. 31.9 mmol, 56%) as a gray solid;

1. additionAfter the addition
2. customThe reaction was quenched
3. additionby pouring the mixture slowly onto ice
4. extractionThe separated, aqueous phase was extracted with chloroform (3×)
5. washThe combined organic phase was washed sequentially with a saturated, aqueous sodium chloride solution (2×) and water
6. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo

ORD record

ord-454d07b0abb14def93e86a2a0fecf95b

Source dataset

uspto-grants-2005_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06894061B2