تفاعل #2615

ord-579f2de7dc1447cc98ef05252e3642bd

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted with chloroform
  2. 2
    غسيلThe resulting organic layer was washed with saturated sodium chloride aqueous solution and water in that order
  3. 3
    تجفيفdried on anhydrous sodium sulfate
  4. 4
    أخرىThereafter, the solvent was removed by evaporation
  5. 5
    أخرىthe resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1) and recrystallization (ethyl acetate-ether)

الإجراء التجريبي

4-Amino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(3-pyridyl)benzamide (225.3 mg, 0.50 mmol) was dissolved in methylene chloride (2.0 ml) to which were subsequently added pyridine (0.05 ml, 0.62 mmol) and benzoyl chloride (0.09 ml, 0.77 mmol). After 14 hours of stirring at room temperature, the reaction solution was mixed with saturated sodium bicarbonate aqueous solution and extracted with chloroform. The resulting organic layer was washed with saturated sodium chloride aqueous solution and water in that order, and dried on anhydrous sodium sulfate. Thereafter, the solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1) and recrystallization (ethyl acetate-ether) to obtain 196.3 mg (70.6%) of the title compound in a light brown powder form.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728835uspto-grants-1998_03