Imidazole → Benzonitrile, 2-fluoro-4-(1H-imidazol-1-ylmethyl)-

HRID 379037

반응식

HRID 379037 반응식
Br[CH2:2][C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[C:5]([F:11])[CH:4]=1.[NH:12]1[CH:16]=[CH:15][N:14]=[CH:13]1>CN(C=O)C>[F:11][C:5]1[CH:4]=[C:3]([CH2:2][N:12]2[CH:16]=[CH:15][N:14]=[CH:13]2)[CH:10]=[CH:9][C:6]=1[C:7]#[N:8]

참가 물질

4

실험 절차

4-Bromomethyl-2-fluoro-benzonitrile (3.44 g, 16.0 mmol) and imidazole (5.47 g, 80.3 mmol) were dissolved in DMF (40 mL) and stirred at ambient temperature for 2 h. The DMF was removed in vacuo and the residue was partitioned between EtOAc (300 mL) and aqueous saturated NaHCO3 solution. The organic layer was separated, washed with NaHCO3 solution, H2O, brine, and dried (MgSO4). Filtration and concentration to dryness gave the title compound after chromatography (silica gel, 1-2% CH3OH/CH2Cl2).

후처리

  1. customThe DMF was removed in vacuo
  2. customthe residue was partitioned between EtOAc (300 mL) and aqueous saturated NaHCO3 solution
  3. customThe organic layer was separated
  4. washwashed with NaHCO3 solution, H2O, brine
  5. dry with materialdried (MgSO4)
  6. filtrationFiltration and concentration to dryness

출처 및 근거

ORD 기록
ord-6172a76ce1384a90bbceeb45ea67674d
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06297239B1

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