تفاعل #5563

ord-4e2651d7658c4004854f8e9660ba034f

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooling
  2. 2
    workup.STIRRINGthe mixture was further stirred under ice-
  3. 3
    درجة الحرارةcooling for 10 minutes
  4. 4
    غسيلThe reaction mixture was washed with water
  5. 5
    استخلاصthe aqueous layer was extracted with methylene chloride (30 ml×3)
  6. 6
    تجفيفdried over anhydrous magnesium sulfate
  7. 7
    workup.DISTILLATIONThen, the solvent was distilled off

الإجراء التجريبي

To a solution of 5-[3-(hydroxy)propylthio]imidazo[1,2-a]pyridine (2.003 g, 9.62 mmoles) and triethylamine (2.01 ml, 14.4 mmoles) in methylene chloride (30 ml) was added methanesulfonyl chloride (0.89 ml, 12 mmoles) with stirring under ice-cooling and the mixture was further stirred under ice-cooling for 10 minutes. The reaction mixture was washed with water and the aqueous layer was extracted with methylene chloride (30 ml×3). The methylene chloride layers were combined and dried over anhydrous magnesium sulfate. Then, the solvent was distilled off to obtain crude 5-[3-(methanesulfonyloxy)propylthio]imidazo[1,2-a]pyridine as a yellow oily product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05244908uspto-grants-1993_09