Potassium Nitrate → Methyl [3-(chlorosulfonyl)phenyl]acetate

Temperatur

0 °C

Methyl 2-(3-mercaptophenyl)acetate (0.55 g, 3.0 mmol) was dissolved in 10 mL acetonitrile and potassium nitrate (0.76 g, 7.5 mmol) was added and the reaction mixture cooled to 0° C. To this suspension sulfuryl chloride was added (0.6 mL, 7.5 mmol) at 0° C. and the reaction mixture was let warm to room temperature and stirred overnight. A solution of saturated sodium bicarbonate was added followed by ethyl acetate (100 mL each). The organic layer was washed with brine, dried over sodium sulfate and concentrated to afford methyl 2-(3-chlorosulfonylphenyl)acetate as an oil (0.59 g, 2.4 mmol, 79% yield). 1H NMR (CDCl3) 7.91 ppm, 2H, m; 7.60 ppm, 1H, d; 7.53 ppm, 1H, t; 3.73 ppm, 2H, s; 3.72 ppm, 3H, s.

1. temperaturethe reaction mixture was let warm to room temperature
2. washThe organic layer was washed with brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated

ORD-Eintrag

ord-08aff3d6ddee47f89a330fbb070def5f

Quelldatensatz

uspto-grants-2009_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07531556B2