تفاعل #41673

ord-2541684330a54406917d1890e9fc82c6

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe reaction liquid
  2. 2
    أخرىThe reaction liquid
  3. 3
    workup.ADDITIONwas poured into a mixture of ice-aqueous saturated sodium bicarbonate
  4. 4
    استخلاصextracted with chloroform
  5. 5
    تجفيفdried with anhydrous sodium carbonate
  6. 6
    أخرىThe solvent was evaporated away under reduced pressure
  7. 7
    أخرىthe resulting residue was purified
  8. 8
    أخرىthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=20/1)

الإجراء التجريبي

1 ml of fuming nitric acid was added to 70 mg of N-(4-(1-acetyl-3-methylpyrrolidin-2-yl)-3-fluorophenyl)pyridine-2-carboxamide, and the reaction liquid was stirred at room temperature for 2 hours. The reaction liquid was poured into a mixture of ice-aqueous saturated sodium bicarbonate, extracted with chloroform, and dried with anhydrous sodium carbonate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=20/1) to obtain the entitled compound as a yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07728025B2uspto-grants-2010_06