Water → 3-Fluoro-4'-hydroxy-1,1'-biphenyl-4-carbonitrile

HRID 466484ノート

反応式

HRID 466484 の反応式
B(Br)(Br)Br.[C:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:18]=[CH:17][C:16]([O:19]C)=[CH:15][CH:14]=2)=[CH:9][C:8]=1[F:21])#[N:6].O>ClCCl>[C:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=2)=[CH:9][C:8]=1[F:21])#[N:6]

参加物

5

反応物 3

HCID 962WaterHCID 25134Boron tribromideHCID 27633572-fluoro-4-(4-methoxyphenyl)benzonitrile

生成物 1

HCID 150656453-Fluoro-4'-hydroxy-1,1'-biphenyl-4-carbonitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of boron tribromide (12.0 ml, 31.8 g, 0.13 mol) in dry dichloromethane (100 ml) was added dropwise to a stirred, cooled (-78° C.) solution of compound 4 (14.0 g, 0.06 mol) in dry dichloromethane (250 ml) under dry nitrogen. The stirred mixture was allowed to warm. to room temperature over 20 h (i.e., until glc analysis revealed absence of starting material). Water was added and a yellow precipitate was produced. The product was extracted into ether (twice), and the combined ethereal extracts were washed with water and dried (MgSO4). The solvent was removed in vacuo to afford a pale-yellow powder.

後処理

  1. temperatureto warm
  2. customa yellow precipitate was produced
  3. extractionThe product was extracted into ether (twice), and the combined ethereal extracts
  4. washwere washed with water
  5. dry with materialdried (MgSO4)
  6. customThe solvent was removed in vacuo
  7. customto afford a pale-yellow powder

出典と根拠

ORDレコード
ord-44de8140876e4c7699fabb2788d9ec39
出典データセット
uspto-grants-1992_10
特許番号
US05156763

反応ノート

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