Potassium Fluoride → 2-Chloro-4,5-difluorobenzonitrile

HRID 1729485

反応式

HRID 1729485 の反応式
[Cl:1][C:2]1[CH:9]=[C:8](Cl)[C:7]([F:11])=[CH:6][C:3]=1[C:4]#[N:5].[F-:12].[K+]>CS(C)=O>[Cl:1][C:2]1[CH:9]=[C:8]([F:12])[C:7]([F:11])=[CH:6][C:3]=1[C:4]#[N:5]

参加物

4

反応物 2

HCID 522689Potassium FluorideHCID 27827532,4-Dichloro-5-fluorobenzonitrile

生成物 1

HCID 40858492-Chloro-4,5-difluorobenzonitrile収率 68.6%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixture comprising 5.70 g (0.03 mol) of 2,4-dichloro-5-fluorobenzonitrile, 3.48 g (0.06 mol) of spray dried KF and 30 ml of dimethylsulfoxide, was reacted at a temperature of from 140° to 150° C. for 3.5 hours in a glass reactor. After completion of the reaction, the mixture was poured into ice water (50 ml) and extracted with chloroform. The chloroform extract was washed five times with water and then dried. Then chloroform was distilled off. The residue was distilled under reduced pressure to obtain 3.57 g (yield: 68.6%) of 2-chloro-4,5-difluorobenzonitrile. Boiling point: 105°-107° C./37 mmHg; melting point: 35°-37° C.

後処理

  1. customAfter completion of the reaction
  2. extractionextracted with chloroform
  3. extractionThe chloroform extract
  4. washwas washed five times with water
  5. customdried
  6. distillationThen chloroform was distilled off
  7. distillationThe residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-6bc9dc00baca4272a4c1fb4f5e1ef79e
出典データセット
uspto-grants-1994_07
特許番号
US05332851

関連ノート

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