Hydroxylamine HCl → 2,2,2-Trifluoro-1-(2,4,6-trimethylphenyl)-ethanone oxime

HRID 1384774ノート

反応式

HRID 1384774 の反応式
[F:1][C:2]([F:15])([F:14])[C:3]([C:5]1[C:10]([CH3:11])=[CH:9][C:8]([CH3:12])=[CH:7][C:6]=1[CH3:13])=O.[Cl-].[OH:17][NH3+:18].C([O-])(=O)C.[Na+]>C(O)C.O>[F:1][C:2]([F:15])([F:14])[C:3]([C:5]1[C:10]([CH3:11])=[CH:9][C:8]([CH3:12])=[CH:7][C:6]=1[CH3:13])=[N:18][OH:17]

参加物

6

反応物 3

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 5205212,2,2-Trifluoro-2',4',6'-trimethylacetophenone

生成物 1

HCID 734559532,2,2-Trifluoro-1-(2,4,6-trimethylphenyl)-ethanone oxime収率 28.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

6.3 g (0.029 mol) of 2,2,2-trifluoro-1-(2,4,6-trimethylphenyl)-ethanone are dissolved in 30 ml of ethanol at 80° C. To the solution are added dropwise 2.0 g (0.029 mol) of hydroxylammonium chloride and 4.1 g (0.050 mol) of sodium acetate dissolved in 15 ml of water. The reaction mixture is refluxed overnight, poured into ice water, and extracted with ethyl acetate. The organic phase is washed with brine, dried over MgSO4, and concentrated. The residue is purified by recrystallization from 20 ml of hexane, yielding 1.9 g of 2,2,2-trifluoro-1-(2,4,6-trimethylphenyl)-ethanone oxime in the form of white crystals, mp. 119-125° C.

後処理

  1. temperatureThe reaction mixture is refluxed overnight
  2. extractionextracted with ethyl acetate
  3. washThe organic phase is washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customThe residue is purified by recrystallization from 20 ml of hexane

出典と根拠

ORDレコード
ord-d89845f3d2d24424ade7802c9fdd4734
出典データセット
uspto-grants-2001_07
特許番号
US06261738B1

反応ノート

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