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

HRID 1019252
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HRID 1019252 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether
용매
HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-16ad6f996315469893c3c80f577a692e
출처 데이터셋
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06486189B2

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