反应详情

温度

60 °C

4-(2-bromo-phenylsulfanyl)-3-sulfino-benzoic acid (14 g, 38 mmol) was added slowly to a stirred solution of methanesulphonic acid (160 ml). The purple solution was heated to 60° C. for 3 hours. The reaction was cooled down to room temperature and was poured into ice (300 ml) where an off-white precipitate appeared. The solid was filtered and washed with water (100 ml) and then dried in a vacuum dessicator over activated silica (9.48 g, 73%). 1HNMR (300MHz, CDCl3): δH=7.29 (1H, t), 7.59 (1H, dd), 7.70 (1H,dd) 7.74 (1H, d), 7.87 (1H, dd), 8.03 (1H, d).m/z (LC-MS, ESP), RT=4.99 min, M−−1)=339

1. temperatureThe reaction was cooled down to room temperature
2. filtrationThe solid was filtered
3. washwashed with water (100 ml)
4. customdried in a vacuum dessicator over activated silica (9.48 g, 73%)