2-Fluorobenzoyl chloride → 2-[1-(2-Fluorobenzoyl)-4,5-dimethyl-1H-imidazol-2-yl]-1-(2-fluorophenyl)ethenyl 2-fluorobenzoate

HRID 1610825ノート

反応式

HRID 1610825 の反応式
[CH3:1][C:2]1[NH:3][C:4]([CH3:8])=[C:5]([CH3:7])[N:6]=1.[F:9][C:10]1[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=1[C:12](Cl)=[O:13]>C(#N)C>[F:9][C:10]1[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=1[C:12]([O:13][C:12]([C:11]1[CH:15]=[CH:16][CH:17]=[CH:18][C:10]=1[F:9])=[CH:1][C:2]1[N:3]([C:12](=[O:13])[C:11]2[CH:15]=[CH:16][CH:17]=[CH:18][C:10]=2[F:9])[C:4]([CH3:8])=[C:5]([CH3:7])[N:6]=1)=[O:13]

参加物

4

反応物 2

HCID 98082-Fluorobenzoyl chlorideHCID 699762,4,5-Trimethylimidazole

生成物 1

HCID 695894172-[1-(2-Fluorobenzoyl)-4,5-dimethyl-1H-imidazol-2-yl]-1-(2-fluorophenyl)ethenyl 2-fluorobenzoate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
0 °C

実験手順

3.00 g (27.23 mmol) 2,4,5-trimethyl-1H-imidazol and 9.37 g (92.59 mmol) TEA are dissolved in 50 ml acetonitrile and cooled to 0° C. 14.25 g (89.87 mmol) 2-fluoro-benzoylchloride are added dropwise and the mixture is stirred 2 h at RT and let stand overnight. The solvent is removed under vacuum, the residue is dissolved in toluene and washed twice with water. The organic phase is filtered through Tonsil (K60) and concentrated under vacuum. The product is used without further purification.

後処理

  1. waitlet stand overnight
  2. customThe solvent is removed under vacuum
  3. dissolutionthe residue is dissolved in toluene
  4. washwashed twice with water
  5. filtrationThe organic phase is filtered through Tonsil (K60)
  6. concentrationconcentrated under vacuum
  7. customThe product is used without further purification

出典と根拠

ORDレコード
ord-f1169e002d6341e795cbecafdb26e692
出典データセット
uspto-grants-2006_01
特許番号
US06984646B2

反応ノート

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