Fluretofene → 4'-Ethenyl-2-fluoro-1,1'-biphenyl

HRID 2398319ノート

反応式

HRID 2398319 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[F:15])=[CH:5][CH:4]=1)#[CH:2].[H][H]>[Pd].N1C=CC=CC=1>[F:15][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[C:6]1[CH:5]=[CH:4][C:3]([CH:1]=[CH2:2])=[CH:8][CH:7]=1

参加物

5

反応物 2

HCID 42040FluretofeneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 194261784'-Ethenyl-2-fluoro-1,1'-biphenyl

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 1049Pyridine溶媒

実験手順

1-Ethynyl-4-(2-fluorophenyl)benzene, 29.6 g., was reduced in a Parr Instrument Company Series 3910 Low-Pressure Shaker-Type Apparatus, using 450 ml. of pyridine, and 0.3 g. of 5 percent palladium on barium sulfate; reduction was carried out at room temperature for 30 minutes and at an initial hydrogen pressure of 30 psig. The reaction mixture was filtered and the filtrate was evaporated in vacuo. The residue was vacuum distilled to give 20.5 g. of solid which was recrystallized from methanol to give 4-(2-fluorophenyl)-1-vinylbenzene, mp 38° . The material contained traces of pyridine and 1-ethyl-4-(2-fluorophenyl)benzene, as shown by nuclear magnetic resonance analysis. The following elemental analysis was obtained:

後処理

  1. filtrationThe reaction mixture was filtered
  2. customthe filtrate was evaporated in vacuo
  3. distillationdistilled
  4. customto give 20.5 g
  5. customof solid which was recrystallized from methanol

出典と根拠

ORDレコード
ord-4faf20f675ff4a92b5154a4768bc0afb
出典データセット
uspto-grants-1977_05
特許番号
US04024284

反応ノート

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