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

HRID 1729485

반응식

HRID 1729485 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 40858492-Chloro-4,5-difluorobenzonitrile수율 68.6%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6bc9dc00baca4272a4c1fb4f5e1ef79e
출처 데이터셋
uspto-grants-1994_07
특허 번호
US05332851

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