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

HRID 379037

反応式

HRID 379037 の反応式
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]

参加物

4

反応物 2

HCID 795ImidazoleHCID 27784664-Cyano-3-fluorobenzyl bromide

生成物 1

HCID 21697068Benzonitrile, 2-fluoro-4-(1H-imidazol-1-ylmethyl)-

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-6172a76ce1384a90bbceeb45ea67674d
出典データセット
uspto-grants-2001_10
特許番号
US06297239B1

関連ノート

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