反应详情

温度

50 °C

150 g (604 mmol) of 3-(pentafluoro-λ6-sulphanyl)benzoic acid [lit. e.g.: C. Zarantonello et al., J. Fluorine Chem. 2007, 128 (12), 1449-1453; WO 2005/047240-A1; also available commercially] were initially charged in 300 ml of trifluoroacetic acid, and 90 ml of concentrated sulphuric acid were added. 161.4 g (907 mmol) of N-bromosuccinimide (NBS) were added to the resulting clear solution. The reaction mixture was then stirred at a temperature of 50° C. overnight (about 18 h). After cooling to RT, the mixture was carefully stirred into about 2.25 liters of ice water. The precipitated product was filtered off with suction, washed with water and dried under high vacuum. This gave 193 g (96% of theory, 98% pure) of the title compound.

1. temperatureAfter cooling to RT
2. filtrationThe precipitated product was filtered off with suction
3. washwashed with water
4. customdried under high vacuum