Hydroxylamine HCl → HCID 73455958、化合物

HRID 1636016ノート

反応式

HRID 1636016 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[C:10]([CH3:11])=[CH:9][CH:8]=[CH:7][C:6]=1C)=O.[Cl-].[OH:16][NH3+:17].[C:18]([O-])(=O)C.[Na+]>C(O)C.O>[F:14][C:2]([F:1])([F:13])[C:3]([C:5]1[CH:6]=[CH:7][C:8]([CH3:18])=[CH:9][C:10]=1[CH3:11])=[N:17][OH:16]

参加物

6

反応物 3

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 186745371-(2,6-Dimethylphenyl)-2,2,2-trifluoroethan-1-one

生成物 1

HCID 73455958HCID 73455958、化合物収率 88.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

12.6 g (0.062 mol) of 2,2,2-trifluoro-1-(2,6-dimethylphenyl)-ethanone are dissolved in 30 ml of ethanol at 80° C. To the solution are added dropwise 4.6 g (0.066 mol) of hydroxylammonium chloride and 8.7 g (0.106 mol) of sodium acetate dissolved in 15 ml of water. The reaction mixture is refluxed overnight, affording white precipitation. The mixture is poured into ice water, and extracted with ethyl acetate. The organic phase is washed with water, NH4Cl aq, and brine, dried over MgSO4, and concentrated, yielding 11.9 g of crude 2,2,2-trifluoro-1-(2,4-dimethylphenyl)-ethanone oxime as a colorless liquid. The crude product is used in the next reaction step without further purification.

後処理

  1. temperatureThe reaction mixture is refluxed overnight
  2. customaffording white
  3. customprecipitation
  4. additionThe mixture is poured into ice water
  5. extractionextracted with ethyl acetate
  6. washThe organic phase is washed with water, NH4Cl aq, and brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-7c0bee1dc5584a8593ed51b729c955da
出典データセット
uspto-grants-2003_01
特許番号
US06512020B1

反応ノート

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