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

HRID 68319

反応式

HRID 68319 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-408cfd8f82b84c36a51f220cd42224fb
出典データセット
uspto-grants-2014_09
特許番号
US08822414B2

関連ノート

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