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Methanol → 1-methyl-6-nitro-1,8-naphthyridin-2(1H)-one

HRID 1620077
ノート
印刷プレビュー

反応式

HRID 1620077 の反応式
C[O-].[Na+].CO.[CH3:6][NH:7][C:8]1[C:13]([CH:14]=[CH:15][C:16](OCCCC)=[O:17])=[CH:12][C:11]([N+:23]([O-:25])=[O:24])=[CH:10][N:9]=1>O>[CH3:6][N:7]1[C:8]2[C:13](=[CH:12][C:11]([N+:23]([O-:25])=[O:24])=[CH:10][N:9]=2)[CH:14]=[CH:15][C:16]1=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 77522859n-Butyl 3-(2-(methylamino)-5-nitropyridin-3-yl)acrylate

生成物 1

HCID 866838621-methyl-6-nitro-1,8-naphthyridin-2(1H)-one収率 76%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5M sodium methoxide (methanol solution) (0.5 ml) was added to a methanol solution (2 ml) containing n-butyl 3-(2-(methylamino)-5-nitropyridin-3-yl)acrylate (43 mg) obtained in the 1st step, followed by reflux for 3.5 hours. Water was added to the reaction solution, followed by extraction with ethyl acetate. The resultant was washed with saturated saline and dried over anhydrous sodium sulfate. Subsequently, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=4:1 to 2:1), and a white solid of 1-methyl-6-nitro-1,8-naphthyridin-2(1H)-one (24 mg) was thus obtained.

後処理

  1. customobtained in the 1st step
  2. temperatureby reflux for 3.5 hours
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe resultant was washed with saturated saline
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationSubsequently, the solvent was distilled away under reduced pressure
  7. customthe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=4:1 to 2:1)

出典と根拠

ORDレコード
ord-5b61e08cb81841a79810af58f048bc88
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772320B2

反応ノート

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