Nitric Acid → N-(4-(1-acetyl-3-methylpyrrolidin-2-yl)-5-fluoro-2-nitrophenyl)pyridine-2-carboxamide

HRID 13395

반응식

HRID 13395 반응식
[N+:1]([O-:4])(O)=[O:2].[C:5]([N:8]1[CH2:12][CH2:11][CH:10]([CH3:13])[CH:9]1[C:14]1[CH:19]=[CH:18][C:17]([NH:20][C:21]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=2)=[O:22])=[CH:16][C:15]=1[F:29])(=[O:7])[CH3:6]>>[C:5]([N:8]1[CH2:12][CH2:11][CH:10]([CH3:13])[CH:9]1[C:14]1[C:15]([F:29])=[CH:16][C:17]([NH:20][C:21]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=2)=[O:22])=[C:18]([N+:1]([O-:4])=[O:2])[CH:19]=1)(=[O:7])[CH3:6]

참가 물질

3

실험 절차

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.

후처리

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. additionwas poured into a mixture of ice-aqueous saturated sodium bicarbonate
  4. extractionextracted with chloroform
  5. dry with materialdried with anhydrous sodium carbonate
  6. customThe solvent was evaporated away under reduced pressure
  7. customthe resulting residue was purified
  8. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=20/1)

출처 및 근거

ORD 기록
ord-2541684330a54406917d1890e9fc82c6
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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