تفاعل #444360

ord-f6ee540821f54bca807c65a8500ed55c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةby refluxing for 20 hours
  2. 2
    درجة الحرارةAfter the reaction mixture was cooled
  3. 3
    workup.DISTILLATIONthe solvent was distilled off
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane
  5. 5
    غسيلwashed with water
  6. 6
    أخرىdried
  7. 7
    workup.DISTILLATIONafter which the solvent was distilled off
  8. 8
    أخرىThe residue was purified by column chromatography (eluent, n-hexane/ethyl acetate 3/1→ethyl acetate)
  9. 9
    أخرىThe resulting residue was crystallized from n-hexane

الإجراء التجريبي

To a solution of 1.527 g (5.0 mmol) of 3-[4-(imidazo[1,2-a]pyridin-5-ylthio)butyl]oxazolidine-2,4-dione and 1.11 ml (5.0 mmol) of decanal in 20 ml of ethanol, 0.04 ml (0.5 mmol) of pyrrolidine was added, followed by refluxing for 20 hours. After the reaction mixture was cooled, the solvent was distilled off. The residue was dissolved in dichloromethane, washed with water and dried, after which the solvent was distilled off. The residue was purified by column chromatography (eluent, n-hexane/ethyl acetate 3/1→ethyl acetate). The resulting residue was crystallized from n-hexane to yield 0.13 g (5.8%, white crystal) of the desired product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05840732uspto-grants-1998_11