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

HRID 1454700노트

반응식

HRID 1454700 반응식
[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]

참가 물질

5

반응물 4

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d1df58d3837d4bef83118b17c5fad2e8
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07479564B2

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