反应 #53542

反应方程式

iodine monochloride

4-fluoro-2-(4′-aminophenyl)benzothiazole

→

4-Fluoro-2-(4′-amino-3′-iodophenyl)benzothiazole

溶剂

acetic acid

acetic acid

反应条件

后处理

1. 1
   其他the solvent was removed under vacuum
2. 2
   workup.DISSOLUTIONThe residue was dissolved in chloroform (100 ml)
3. 3
   洗涤washed with aqueous sodium carbonate (50 ml), aqueous sodium thiosulfate (50 ml) and water (50 ml)
4. 4
   其他Evaporation of the solvent
5. 5
   其他followed by column chromatography (chloroform) and recrystallization from methanol
6. 6
   其他gave pale cream needles

实验过程

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.

来源