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Hydrochloric Acid → 2-Chloro-4,5-difluorobenzoic acid

HRID 2371573
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HRID 2371573 반응식
C[C:2]([C:4]1[C:9]([Cl:10])=[CH:8][C:7]([F:11])=[C:6]([F:12])[CH:5]=1)=[O:3].Cl[O-:14].[Na+].Cl>C(Cl)Cl>[Cl:10][C:9]1[CH:8]=[C:7]([F:11])[C:6]([F:12])=[CH:5][C:4]=1[C:2]([OH:3])=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 27364892'-Chloro-4',5'-difluoroacetophenoneHCID 23665760Sodium Hypochlorite

생성물 1

HCID 7371712-Chloro-4,5-difluorobenzoic acid수율 85.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To 19.1 g (0.1 mol) of 2-chloro-4,5-difluoroacetophenone, 280.4 g (0.4 mol) of a 12% sodium hypochlorite aqueous solution was added, and the mixture was reacted under reflux for 4 hours. After cooling, concentrated hydrochloric acid was dropwise added thereto until the pH became 1. The formed white crystals were dissolved in methylene chloride and separated from the aqueous phase. The separated aqueous phase was extracted twice with methylene chloride, and the extracts were added to the oil phase. Then, the solvent was distilled off to obtain 16.4 g (yield: 85.1%) of 2-chloro-4,5-difluorobenzoic acid as white crystal.

후처리

  1. customthe mixture was reacted
  2. temperatureunder reflux for 4 hours
  3. temperatureAfter cooling
  4. customseparated from the aqueous phase
  5. extractionThe separated aqueous phase was extracted twice with methylene chloride
  6. additionthe extracts were added to the oil phase
  7. distillationThen, the solvent was distilled off

출처 및 근거

ORD 기록
ord-006c97973f1a44b89d2a27c718de8fd7
출처 데이터셋
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05093515

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