N-methylhydroxylamine hydrochloride → 1-(2-thienyl)-2-(1H-imidazol-1-yl)-N-methylethanimine N-oxide

HRID 622184

反応式

HRID 622184 の反応式
[N:1]1([CH2:6][C:7]([C:9]2[S:10][CH:11]=[CH:12][CH:13]=2)=O)[CH:5]=[CH:4][N:3]=[CH:2]1.Cl.[CH3:15][NH:16][OH:17].C([O-])(=O)C.[Na+]>C(O)C>[N:1]1([CH2:6][C:7]([C:9]2[S:10][CH:11]=[CH:12][CH:13]=2)=[N+:16]([O-:17])[CH3:15])[CH:5]=[CH:4][N:3]=[CH:2]1

参加物

5

反応物 3

HCID 77906N-methylhydroxylamine hydrochlorideHCID 517045Sodium AcetateHCID 142647511-(2-thienyl)-2-(1H-imidazol-1-yl)ethanone

生成物 1

HCID 855509281-(2-thienyl)-2-(1H-imidazol-1-yl)-N-methylethanimine N-oxide収率 89.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

Under a nitrogen, a mixture of 22.00 g (0.114 mol) of 2-(1H-imidazol-1-yl)-1-(2-thienyl)ethanone (3), 11.49 g (0.138 mol) of N-methylhydroxylamine hydrochloride, and 22.55 g (0.275 mol) of sodium acetate in 250 ml of ethanol is heated to 50° C. and stirred for 4 days. The reaction mixture is filtered while hot and the filtrate concentrated in vacuo. Crystallization from ethanol gives 22.62 g (89%) of compound 4, melting point 162°-164° C. Anal. Calcd. for C10H11N3OS: C, 54.28; H, 5.01; N, 18.99. Found: C, 54.16; H, 5.06; N, 18.86.

後処理

  1. filtrationThe reaction mixture is filtered while hot and the filtrate
  2. concentrationconcentrated in vacuo
  3. customCrystallization from ethanol

出典と根拠

ORDレコード
ord-d7dcb093938440049d0a63ee78fc3d4b
出典データセット
uspto-grants-1988_09
特許番号
US04769470

関連ノート

読み込み中…