反应详情

温度

140 °C

2-Bromobenzenethiol (25 g, 132 mmol) was added to a solution of 4-fluoro-3-sulfino-benzoic acid (13.5 g, 66 mmol) and NaOH pellets (11 g, 264 mmol) in water (30 ml). The yellow mixture was then degassed for 10 minutes and then heated to 140° C. for 48 hours. The reaction was then cooled to 0° C. and acidified to pH 4–5 (pH paper) with concentrated HCl. The precipitate formed was filtered, washed with hexane and was dried in a vacuum dessicator over activated silica overnight (20.69 g, 84%). m/z (LC-MS, ESP), RT=3.67 min, (M−−1)=373.

1. customThe yellow mixture was then degassed for 10 minutes
2. temperatureThe reaction was then cooled to 0° C.
3. customThe precipitate formed
4. filtrationwas filtered
5. washwashed with hexane
6. customwas dried in a vacuum dessicator over activated silica overnight (20.69 g, 84%)