Thionyl Chloride → 3-Bromo-4-fluorobenzonitrile

HRID 851287

反応式

HRID 851287 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[F:11])[C:5]([NH2:7])=O.S(Cl)(Cl)=O>>[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[F:11])[C:5]#[N:7]

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 27733293-bromo-4-fluorobenzamide

生成物 1

HCID 1235793-Bromo-4-fluorobenzonitrile収率 91%

実験手順

765 g (3.5 moles) of 3-bromo-4-fluoro-benzoic acid amide was added, at 25° C., to 1,150 g (9.7 moles) of thionyl chloride and the mixture was heated under reflux at 85° to 90° C., while stirring, until virtually no further evolution of gas took place. The excess thionyl chloride was then distilled off and the residue was fractionated in a short column. 630 g (91% of theory) of 3-bromo-4-fluoro-benzonitrile with a boiling point of 115°-116° C./20 mm Hg were obtained.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux at 85° to 90° C.
  3. distillationThe excess thionyl chloride was then distilled off

出典と根拠

ORDレコード
ord-389ca1d4043b4210994934deab942952
出典データセット
uspto-grants-1983_05
特許番号
US04383949

関連ノート

読み込み中…