Water → HCID 178502684、化合物

HRID 2368469ノート

反応式

HRID 2368469 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([C:13]([OH:15])=O)=[CH:11][N:10]=[C:9]2[SH:16])=[CH:4][CH:3]=1.[CH3:17][NH:18][O:19][CH3:20].C(N=C=NCCCN(C)C)C.O>N1C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:12]([C:13]([N:18]([O:19][CH3:20])[CH3:17])=[O:15])=[CH:11][N:10]=[C:9]2[SH:16])=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 14232N,O-DimethylhydroxylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 178524781HCID 178524781、化合物

生成物 1

HCID 178502684HCID 178502684、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 1-(4-fluorophenyl)-2-mercapto-1H-imidazole-5-carboxylic acid (4) (2.2 g, 9.23 mmol), N,O-dimethylhydroxylamine (0.9 g, 9.23 mmol), and 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDCI) (1.77 g, 9.23 mmol) in pyridine was heated at 40° C. overnight. The reaction was cooled to room temperature, water was added and the solution was extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo to yield 1-(4-fluorophenyl)-2-mercapto-N-methoxy-N-methyl-1H-imidazole-5-carboxamide (5) as a light yellow solid.

後処理

  1. extractionthe solution was extracted with ethyl acetate
  2. dry with materialThe combined organic layers were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-ddaa5fe9fc7943caaf773758245c2802
出典データセット
uspto-grants-2014_04
特許番号
US08703776B2

反応ノート

読み込み中…