Hydroxylamine HCl → N-[2,2,2-Trifluoro-1-(4-methoxyphenyl)ethylidene]hydroxylamine

HRID 1384775

反応式

HRID 1384775 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([O: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]([O:11][CH3:12])=[CH:7][CH:6]=1)=[N:17][OH:16]

参加物

6

反応物 3

HCID 21645Hydroxylamine HClHCID 1365552,2,2-Trifluoro-4'-methoxyacetophenoneHCID 517045Sodium Acetate

生成物 1

HCID 59115151N-[2,2,2-Trifluoro-1-(4-methoxyphenyl)ethylidene]hydroxylamine収率 75.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

37.2 g (0.182 mol) of 2,2,2-trifluoro-1-(4-methoxyphenyl)-ethanone are dissolved in 150 ml of ethanol at 80° C. To the solution are added dropwise 13.3 g (0.191 mol) of hydroxylammonium chloride and 25.4 g (0.309 mol) of sodium acetate dissolved in 75 ml of water. The reaction mixture is refluxed for 4 hours. The mixture is poured into ice water, the precipitate is filtered, yielding 30.0 g of 2,2,2-trifluoro-1-(4-methoxyphenyl)-ethanone oxime as a pale 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 4 hours
  2. filtrationthe precipitate is filtered

出典と根拠

ORDレコード
ord-5033cf721aa644cdada4ae0fae2a0bed
出典データセット
uspto-grants-2001_07
特許番号
US06261738B1

関連ノート

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