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

HRID 622184

반응식

HRID 622184 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-d7dcb093938440049d0a63ee78fc3d4b
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04769470

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