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

HRID 13395

反応式

HRID 13395 の反応式
[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]

参加物

3

反応物 2

HCID 944Nitric AcidHCID 23145589N-(4-(1-acetyl-3-methylpyrrolidin-2-yl)-3-fluorophenyl)pyridine-2-carboxamide

生成物 1

HCID 23145679N-(4-(1-acetyl-3-methylpyrrolidin-2-yl)-5-fluoro-2-nitrophenyl)pyridine-2-carboxamide

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-2541684330a54406917d1890e9fc82c6
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

関連ノート

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