Ethanol → Ethyl 2-(5-aminopyridin-2-yl)acetate

HRID 1454700ノート

反応式

HRID 1454700 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[N:6][CH:7]=1.OS(O)(=O)=O.C([O-])(O)=O.[Na+].[CH2:22](O)[CH3:23]>>[CH2:22]([O:10][C:9](=[O:11])[CH2:8][C:5]1[CH:4]=[CH:3][C:2]([NH2:1])=[CH:7][N:6]=1)[CH3:23]

参加物

5

反応物 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 218763062-(5-Aminopyridin-2-yl)acetic acid

生成物 1

HCID 21876034Ethyl 2-(5-aminopyridin-2-yl)acetate

実験手順

To a solution of (5-amino-2-pyridinyl)acetic acid (1.46 g, 9.6 mmol, Daisley; R. W.; Hanbali, J. R., Synthetic Communications., 1981, 11(9), 743.) in ethanol was added conc. H2SO4 and stirred for 16.5 h under hydrogen atmosphere at room temperature. The mixture was neutralized with saturated NaHCO3 aqueous solution and the solvent was removed. The mixture was diluted with water and extracted with ethyl acetate (5×20 ml). The organic layer was washed with brine, dried (MgSO4) and concentrated to give 1.2 g of title compound as brown oil.

後処理

  1. customthe solvent was removed
  2. additionThe mixture was diluted with water
  3. extractionextracted with ethyl acetate (5×20 ml)
  4. washThe organic layer was washed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-d1df58d3837d4bef83118b17c5fad2e8
出典データセット
uspto-grants-2009_01
特許番号
US07479564B2

反応ノート

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