تفاعل #6187

ord-efc045dc445b4acca9722be49a0b70c5

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 30 minutes
  3. 3
    غسيلThe reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water
  4. 4
    أخرىdried
  5. 5
    workup.DISTILLATIONThe solvent was distilled off
  6. 6
    أخرىThe residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:10)

الإجراء التجريبي

To a solution of 600 mg (2.49 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 1.39 ml (9.96 mmol) of triethylamine in 25 ml of methylene chloride was added 0.42 ml (2.99 mmol) of hexanoyl chloride under ice-cooling with stirring and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water and dried. The solvent was distilled off. The residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:10) to obtain 542 mg of the desired compound (81.7%, pale yellow oil).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05246948uspto-grants-1993_09