2-Methylbenzimidazole → 1-(3-Bromobenzyl)-2-methylbenzimidazole

HRID 1017782ノート

反応式

HRID 1017782 の反応式
CC(C)([O-])C.[K+].[Br:7][C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][CH:15]=1)[CH2:11]Br.[CH3:16][C:17]1[NH:18][C:19]2[CH:25]=[CH:24][CH:23]=[CH:22][C:20]=2[N:21]=1>CS(C)=O.C(OCC)(=O)C>[Br:7][C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][CH:15]=1)[CH2:11][N:18]1[C:19]2[CH:25]=[CH:24][CH:23]=[CH:22][C:20]=2[N:21]=[C:17]1[CH3:16]

参加物

6

反応物 3

HCID 119842-MethylbenzimidazoleHCID 699793-Bromobenzyl bromideHCID 23665647Potassium tert-butoxide

生成物 1

HCID 169952091-(3-Bromobenzyl)-2-methylbenzimidazole

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

First 1.23 g (11 mmol) of potassium-tert-butoxide and after 45 minutes 2.62 g (10.5 mmol) of 3-bromo-benzylbromide are added to a solution of 1.32 g (10 mmol) of 2-methyl-benzimidazole in 10 ml of absolute dimethylsulphoxide and the reaction mixture is stirred for 4 hours. The mixture is then diluted with ethyl acetate, washed 3× with 14% NaCl solution, dried, concentrated and purified by flash chromatography (silica gel; petroleum ether/ethyl acetate=9:1 to ethyl acetate).

後処理

  1. washwashed 3× with 14% NaCl solution
  2. customdried
  3. concentrationconcentrated
  4. custompurified by flash chromatography (silica gel; petroleum ether/ethyl acetate=9:1 to ethyl acetate)

出典と根拠

ORDレコード
ord-d61d275d49a349a09695d86e9121a3be
出典データセット
uspto-grants-2002_11
特許番号
US06479524B1

反応ノート

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