تفاعل #53542

ord-bbf5a827234a40c89a9494fb927ae3dd

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06858633B1uspto-grants-2005_02