Potassium Carbonate → 3-Amino-2-(1-[3,4-dimethylphenylcarbonylmethyl]benzimidazol-2-yl)-1,2,4-triazole

HRID 553019

反応式

HRID 553019 の反応式
[NH2:1][C:2]1[N:3]([C:7]2[NH:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]=2)[N:4]=[CH:5][N:6]=1.[CH3:16][C:17]1[CH:18]=[C:19]([CH:24]=[CH:25][C:26]=1[CH3:27])[C:20](=[O:23])[CH2:21]Br.C(=O)([O-])[O-].[K+].[K+]>O>[NH2:1][C:2]1[N:3]([C:7]2[N:11]([CH2:21][C:20]([C:19]3[CH:24]=[CH:25][C:26]([CH3:27])=[C:17]([CH3:16])[CH:18]=3)=[O:23])[C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]=2)[N:4]=[CH:5][N:6]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 6082642-(1H-Benzoimidazol-2-YL)-2H-[1,2,4]triazol-3-ylamineHCID 37031132-Bromo-1-(3,4-dimethylphenyl)ethan-1-one

生成物 1

HCID 112332783-Amino-2-(1-[3,4-dimethylphenylcarbonylmethyl]benzimidazol-2-yl)-1,2,4-triazole

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A suspension of 3-amino-2-(1H-benzimidazol-2-yl)-1,2,4-triazole (0.15 g, 0.75 mol), 3,4-dimethyl phenacyl bromide (0.204 g, 0.9 mmol) and dry potassium carbonate (0.258 g, 1.87 mmol) is stirred at room temperature for 16 hours. The mixture is diluted with water and the product extracted with ethyl acetate. The product is purified by chromatography on silicagel. M.p. 190-193° C., 1H-NMR (400 MHz, d6-DMSO): 7.84 (m, 1H); 7.77 (m, 3H); 7.65 (m, 2H); 7.50 (s, 1H); 7.33 (d, 1H); 6.22 (s, 2H); 2.30 (s, 6H).

後処理

  1. extractionthe product extracted with ethyl acetate
  2. customThe product is purified by chromatography on silicagel

出典と根拠

ORDレコード
ord-779d95b0aff54cba9a4dcb97837b3204
出典データセット
uspto-grants-2011_05
特許番号
US07951957B2

関連ノート

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