反应详情

温度

50 °C

To anhydrous 2-picoline (1.05 g, 11 mmol) was slowly added dropwise chlorsulphonic acid (0.26 g, 2.21 mmol) below 10° C. then 2-(4'-amino-3'-iodophenyl)benzothiazole (0.5 g, 2.21 mmol). The mixture was heated to 50° C. with stirring for 1 hour. After leaving to stand for 2 hours at room temperature, 6 ml of 10% aqueous sodium carbonate was added. The resulting mixture was stirred for 40 minutes at room temperature and concentrated under reduced pressure. The precipitate was filtered off, washed carefully with cold water and treated with hot chlorform. Golden crystals were afforded (0.62 g, 85.5%), m.p. 288-290° C.

1. customAfter leaving
2. waitto stand for 2 hours at room temperature
3. stirringThe resulting mixture was stirred for 40 minutes at room temperature
4. concentrationconcentrated under reduced pressure
5. filtrationThe precipitate was filtered off
6. washwashed carefully with cold water
7. additiontreated with hot chlorform
8. customGolden crystals were afforded (0.62 g, 85.5%), m.p. 288-290° C.