Hydroxylamine HCl → Methyl 2-((5-(1-(hydroxyimino)ethyl)pyridin-2-yl)oxy)acetate

HRID 68310

반응식

HRID 68310 반응식
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([O:10][CH2:11][C:12]([O:14][CH3:15])=[O:13])=[N:8][CH:9]=1)(=O)[CH3:2].C([O-])(=O)C.[Na+].[Cl-].[OH:22][NH3+:23]>C(O)C.O>[OH:22][N:23]=[C:1]([C:4]1[CH:5]=[CH:6][C:7]([O:10][CH2:11][C:12]([O:14][CH3:15])=[O:13])=[N:8][CH:9]=1)[CH3:2]

참가 물질

6

반응물 3

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 68281905Methyl 2-((5-acetylpyridin-2-yl)oxy)acetate

생성물 1

HCID 86699620Methyl 2-((5-(1-(hydroxyimino)ethyl)pyridin-2-yl)oxy)acetate수율 88%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a solution of methyl 2-((5-acetylpyridin-2-yl)oxy)acetate (1.23 gm, 0.059 mole) in ethanol (10 mL), a solution of sodium acetate (0.942 gm, 0.0117 mole) and hydroxylammonium chloride (1.2 gm, 0.0117 mole) in water (5 ml) was added and the reaction mixture was refluxed for 1 h. The reaction mixture was coiled to room temperature and solvent was evapourated in vacuum. The residue was diluted with ice cold water and solid seperated was filtered, washed with water and dried over P2O5 under vacuum to yield 1.15 gm (88%) of title product as off white solid.

후처리

  1. temperaturethe reaction mixture was refluxed for 1 h
  2. customwas coiled to room temperature
  3. additionThe residue was diluted with ice cold water and solid
  4. customseperated
  5. filtrationwas filtered
  6. washwashed with water
  7. dry with materialdried over P2O5 under vacuum

출처 및 근거

ORD 기록
ord-c52054b585b049c482cb8432945af5a3
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822414B2

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