Hydroxyamine hydrochloride → HCID 6400952、化合物

HRID 1192820ノート

反応式

HRID 1192820 の反応式
Cl.[NH2:2][OH:3].[CH3:4][NH:5][C:6](=[O:15])[C:7](=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>N1C=CC=CC=1>[OH:3][N:2]=[C:7]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:6]([NH:5][CH3:4])=[O:15]

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 10877451N-methyl-2-oxo-2-phenylacetamide

生成物 1

HCID 6400952HCID 6400952、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Hydroxylamine hydrochloride (5.96 g, 2.5 eq.) was added to a solution of N-methyl-2-oxo-2-phenylacetamide (5.6 g, 34.3 mmol) in pyridine (25 ml). After stirring for 10 h at room temperature, the excess pyridine was removed in vacuo and the residue was taken up in 250 ml of dichloromethane. The organic phase was washed with 200 ml of water and then again with aqueous hydrochloric acid (0.1 M, 250 ml). The precipitated solid was filtered off, giving 2-(hydroxyimino)-N-methyl-2-phenylacetamide as a yellow solid (2.31 g, pure Z isomer). The filtrate was concentrated by evaporation in vacuo. This gave 4.50 g of 2-(hydroxyimino)-N-methyl-2-phenylacetamide (Z/E=mixture of isomers) as a yellow solid.

後処理

  1. customthe excess pyridine was removed in vacuo
  2. washThe organic phase was washed with 200 ml of water
  3. filtrationThe precipitated solid was filtered off

出典と根拠

ORDレコード
ord-3a6b693839be4a0aaf45d529f4caa07e
出典データセット
uspto-grants-2014_03
特許番号
US08680283B2

反応ノート

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