Reaktion #53542

Reaktionsgleichung

iodine monochloride

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

→

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

Lösungsmittel

acetic acid

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe solvent was removed under vacuum
2. 2
   workup.DISSOLUTIONThe residue was dissolved in chloroform (100 ml)
3. 3
   Waschenwashed with aqueous sodium carbonate (50 ml), aqueous sodium thiosulfate (50 ml) and water (50 ml)
4. 4
   SonstigeEvaporation of the solvent
5. 5
   Sonstigefollowed by column chromatography (chloroform) and recrystallization from methanol
6. 6
   Sonstigegave pale cream needles

Vorschrift

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.

Quelle