反应详情

A solution of the 4-fluoro-2-(4′-aminophenyl)benzothiazole prepared as described in Example 3 (4.5 mmol) in acetic acid (20 ml) was added dropwise to a solution of iodine monochloride (5.8 mmol) in acetic acid (20 ml) at 25° C. The resulting solution was stirred for 2 hr, then the solvent was removed under vacuum. The residue was dissolved in chloroform (100 ml) and washed with aqueous sodium carbonate (50 ml), aqueous sodium thiosulfate (50 ml) and water (50 ml). Evaporation of the solvent, followed by column chromatography (chloroform) and recrystallization from methanol gave pale cream needles.

1. customthe solvent was removed under vacuum
2. dissolutionThe residue was dissolved in chloroform (100 ml)
3. washwashed with aqueous sodium carbonate (50 ml), aqueous sodium thiosulfate (50 ml) and water (50 ml)
4. customEvaporation of the solvent
5. customfollowed by column chromatography (chloroform) and recrystallization from methanol
6. customgave pale cream needles