반응 #53542

반응 방정식

iodine monochloride

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

→

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

용매

acetic acid

acetic acid

반응 조건

후처리

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

실험 절차

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.

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