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Hydroxylamine HCl → Diethyl 2,2'-((5-(1-(hydroxyimino)ethyl)oxazol-2-yl)azanediyl)diacetate

HRID 68319
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HRID 68319 반응식
[C:1]([C:4]1[O:8][C:7]([N:9]([CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[N:6][CH:5]=1)(=O)[CH3:2].C([O-])(=O)C.[Na+].[Cl-].[OH:28][NH3+:29]>C(O)C.O>[OH:28][N:29]=[C:1]([C:4]1[O:8][C:7]([N:9]([CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[N:6][CH:5]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 68282007Diethyl 2,2'-((5-acetyloxazol-2-yl)azanediyl)diacetate

생성물 1

HCID 86699627Diethyl 2,2'-((5-(1-(hydroxyimino)ethyl)oxazol-2-yl)azanediyl)diacetate수율 80%

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 962
Water
용매

실험 절차

To a solution of diethyl 2,2′-((5-acetyloxazol-2-yl)azanediyl)diacetate (300 mg, 1.01 mmoles) in ethanol (6 mL), a solution of sodium acetate (165 mg, 2.01 mmoles) and hydroxylammonium chloride (139 mg gm, 2.01 mmoles) in water (2 ml) was added and the reaction mixture was refluxed for 1 h. The reaction mixture was cooled to room temperature and solvent was evapourated in vacuum. The residue was diluted with ice cold water and extracted with ethyl acetate. The combined ethyl acetate extract was washed with water & brine, dried over sodium sulphate and evaporated under reduced pressure to yield 252 mg (80%) of title product as thick liquid.

후처리

  1. temperaturethe reaction mixture was refluxed for 1 h
  2. additionThe residue was diluted with ice cold water
  3. extractionextracted with ethyl acetate
  4. extractionThe combined ethyl acetate extract
  5. washwas washed with water & brine
  6. dry with materialdried over sodium sulphate
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-408cfd8f82b84c36a51f220cd42224fb
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822414B2

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