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3-(Thien-2-yl)benzoic acid → N-[3-(4,5-dimethylimidazol-1-yl)-phenyl]-3-(2-thienyl)benzamide

HRID 1835480
ノート
印刷プレビュー

反応式

HRID 1835480 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][CH:14]=1)[C:9]([OH:11])=O.[CH3:15][C:16]1[N:17]=[CH:18][N:19]([C:22]2[CH:23]=[C:24]([CH:26]=[CH:27][CH:28]=2)[NH2:25])[C:20]=1[CH3:21].Cl.C(N=C=NCCCN(C)C)C>ClCCl.CN(C)C1C=CN=CC=1>[CH3:15][C:16]1[N:17]=[CH:18][N:19]([C:22]2[CH:23]=[C:24]([NH:25][C:9](=[O:11])[C:8]3[CH:12]=[CH:13][CH:14]=[C:6]([C:2]4[S:1][CH:5]=[CH:4][CH:3]=4)[CH:7]=3)[CH:26]=[CH:27][CH:28]=2)[C:20]=1[CH3:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7368613-(Thien-2-yl)benzoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 235036513-(4,5-Dimethylimidazol-1-yl)phenylamine

生成物 1

HCID 23503677N-[3-(4,5-dimethylimidazol-1-yl)-phenyl]-3-(2-thienyl)benzamide収率 62.6%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine
触媒
HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of 3-(2-thienyl)benzoic acid (103 mg) and 3-(4,5-dimethylimidazol-1-yl)aniline (94 mg) in dichloromethane (2 ml) were added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (135 mg) and 4-dimethylaminopyridine (31 mg), and the mixture was stirred for 24 hours. The mixture was diluted with dichloromethane and washed with water and brine. The mixture was dried over magnesium sulfate and evaporated under reduced pressure. The residue was triturated with methanol, and the insoluble material was collected by filtration and dried to give N-[3-(4,5-dimethylimidazol-1-yl)-phenyl]-3-(2-thienyl)benzamide (117 mg, 62.6%).

後処理

  1. washwashed with water and brine
  2. dry with materialThe mixture was dried over magnesium sulfate
  3. customevaporated under reduced pressure
  4. customThe residue was triturated with methanol
  5. filtrationthe insoluble material was collected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-3e926c10f9c94fa28e9370b0c7eea171
出典データセット
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06770667B1

反応ノート

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