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Methyl iodide → 1-[3-(4-Bromobenzyl)-5-chloro-2-phenyl-3H-imidazol-4-yl]ethanol

HRID 1019252
ノート
印刷プレビュー

反応式

HRID 1019252 の反応式
[Br:1][C:2]1[CH:22]=[CH:21][C:5]([CH2:6][N:7]2[C:11]([CH:12]=[O:13])=[C:10]([Cl:14])[N:9]=[C:8]2[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:4][CH:3]=1.[Mg].[CH3:24]I.OS([O-])(=O)=O.[Na+]>C1COCC1.C(OCC)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][N:7]2[C:11]([CH:12]([OH:13])[CH3:24])=[C:10]([Cl:14])[N:9]=[C:8]2[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:21][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6328Methyl iodideHCID 516919Sodium BisulfateHCID 5462224MagnesiumHCID 109157723-(4-Bromobenzyl)-5-chloro-2-phenyl-3H-imidazole-4-carbaldehyde

生成物 1

HCID 184001141-[3-(4-Bromobenzyl)-5-chloro-2-phenyl-3H-imidazol-4-yl]ethanol

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

3.8 g of 3-(4-bromobenzyl)-5-chloro-2-phenyl-3H-imidazole-4-carbaldehyde are dissolved in 50 ml of THF and a Grignard solution, prepared from 385 mg of magnesium turnings and 990 μl of methyl iodide in 50 ml of diethyl ether, is slowly added by syringe at RT. The mixture is stirred at RT for 3 days, then 200 ml of a 5% aqueous NaHSO4 solution are added und the mixture is extracted twice using 200 ml of EA each time. The extract is dried over Na2SO4 and the solvent is removed in vacuo. 3.7 g of a colorless oil are obtained.

後処理

  1. additionis slowly added by syringe at RT
  2. extractionis extracted twice
  3. dry with materialThe extract is dried over Na2SO4
  4. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-16ad6f996315469893c3c80f577a692e
出典データセット
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06486189B2

反応ノート

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