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Methanol → methyl 1,6-naphthyridine-2-carboxylate

HRID 2307247
ノート
印刷プレビュー

反応式

HRID 2307247 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][N:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]([OH:13])=[O:12].OS(O)(=O)=O.[CH3:19]O>>[CH3:19][O:12][C:11]([C:2]1[CH:3]=[CH:4][C:5]2[C:10](=[CH:9][CH:8]=[N:7][CH:6]=2)[N:1]=1)=[O:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 7359081,6-Naphthyridine-2-carboxylic acid

生成物 1

HCID 2761109methyl 1,6-naphthyridine-2-carboxylate

実験手順

To a mixture of 1,6-naphthyridine-2-carboxylic acid (1 g, 5.7 mmol) and 100 mL of methanol was added carefully ˜0.5 mL of conc. H2SO4. The mixture was kept under reflux overnight. The mixture was cooled to room temperature and solvent was evaporated. To the residue was added carefully (carbon dioxide evolution) half saturated sodium bicarbonate solution to neutralize the acid. The mixture was extracted from ethyl acetate (3 times) and the combined organic was washed with brine. After drying over anhydrous MgSO4, solvent was evaporated. The product, 1,6-naphthyridine-2-carboxylic acid methyl ester, (IIIe) was isolated as a solid (932 mg, 87% yield), which was used for the next step without further purification. A mixture of ester (IIIe) (322 mg, 1.71 mmol) and methylacetate (dry, 10 mL) was treated with NaH (60% dispersion in mineral oil, 100 mg, 2.5 mmol) and the resulting mixture was kept under reflux for 2 h, during which a cake formation was noticed. The reaction mixture was cooled to room temperature and solvent was evaporated. The residue was treated ˜20 mL of water. The mixture was neutralized with conc. HCl. A solid was obtained which was filtered, washed (water followed by hexane) and dried. Yield: 158 mg (40%). The product, ethyl 3-oxo-3-pyridino[3,4-e]pyridin-2-yl-propanoate, (Vf) was used for the next step without further purification.

後処理

  1. temperatureunder reflux overnight
  2. customsolvent was evaporated
  3. additionTo the residue was added carefully (carbon dioxide evolution) half saturated sodium bicarbonate solution
  4. extractionThe mixture was extracted from ethyl acetate (3 times)
  5. washthe combined organic was washed with brine
  6. dry with materialAfter drying over anhydrous MgSO4, solvent
  7. customwas evaporated

出典と根拠

ORDレコード
ord-4f4d556d9e5149d3a82da66857c4ec1a
出典データセット
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06831075B2

反応ノート

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