Hydroxylamine HCl → HCID 59115139、化合物

HRID 1384776ノート

反応式

HRID 1384776 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][CH:6]=1)=O.[Cl-].[OH:16][NH3+:17].C([O-])(=O)C.[Na+]>C(O)C.O>[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][CH:6]=1)=[N:17][OH:16]

参加物

6

反応物 3

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 27606164'-Thiomethyl-2,2,2-trifluoroacetophenone

生成物 1

HCID 59115139HCID 59115139、化合物収率 97%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

49.3 g (0.224 mol) of 2,2,2-trifluoro-1-(4-methylthiophenyl)-ethanone are dissolved in 250 ml of ethanol at 80° C. To the solution are added dropwise 16.3 g (0.235 mol) of hydroxylammonium chloride and 31.2 g (0.381 mol) of sodium acetate dissolved in 125 ml of water. The reaction mixture is refluxed for 6.5 hours, and poured into ice water. Filtration of the precipitate yields 51.1 g of 2,2,2-trifluoro-1-(4-methylthiophenyl)-ethanone oxime, as a yellow solid. The crude product is used in the next reaction step without further purification.

後処理

  1. temperatureThe reaction mixture is refluxed for 6.5 hours
  2. filtrationFiltration of the precipitate

出典と根拠

ORDレコード
ord-92474d680c214ab5a533206fa67b8b43
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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