تفاعل #5556

ord-87ae7e60b3f94aeab00f82581b06295a

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooling
  2. 2
    workup.STIRRINGthe mixture was stirred at room temperature for 1 hour
  3. 3
    غسيلThe reaction mixture was washed in turn with an aqueous sodium bicarbonate solution and saturated saline
  4. 4
    تجفيفdried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONAfter the solvent was distilled off
  6. 6
    أخرىthe crude product thus obtained
  7. 7
    أخرىwas recrystallized from methylene-ethanol

الإجراء التجريبي

To a suspension of 5-[3-(amino)propyloxy]imidazo[1,2-a]pyridine dihydrochloride (2.64 g, 10 mmoles) and triethylamine (4.88 ml, 35 mmoles) in methylene chloride (100 ml)-acetonitrile (30 ml) was added benzenesulfonyl chloride (1.53 ml, 12 mmoles) under ice-cooling with stirring and the mixture was stirred at room temperature for 1 hour. The reaction mixture was washed in turn with an aqueous sodium bicarbonate solution and saturated saline and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the crude product thus obtained was recrystallized from methylene-ethanol to obtain 1.97 g of the desired product (59.5%, light brown crystals).

المصدر

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