Sodium percarbonate → 3,4-Difluorobenzoic acid

HRID 374618

반응식

HRID 374618 반응식
[C:1]([O-:4])([O-])=[O:2].C([O-])([O-])=O.OO.OO.OO.[Na+].[Na+].[Na+].[Na+].[F:19][C:20]1[CH:21]=[C:22]([CH:31]=[CH:32][C:33]=1[F:34])C(C1C=CC=CC=1)=O>FC(F)(F)C(O)=O>[F:19][C:20]1[CH:21]=[C:22]([CH:31]=[CH:32][C:33]=1[F:34])[C:1]([OH:4])=[O:2]

참가 물질

4

반응물 2

HCID 159762Sodium percarbonateHCID 5699083,4-Difluorobenzophenone

생성물 1

HCID 991663,4-Difluorobenzoic acid수율 95.5%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

2.5 g of sodium percarbonate were added over 1 h to a solution of 2.2 g (10 mmol) of 3,4-difluorobenzophenone and 20 ml of trifluoroacetic acid (0° C.) and the temperature was then allowed to rise to 20° C. The mixture was stirred for 16 h at this temperature and 50 g of ice were then added. The mixture was subsequently extracted twice with dichloromethane and the organic phases were washed (NaHCO3) until the washings were neutral. The solvent was then removed. Working-up as described in Example 22 gave 1.2 g (7.6 mmol, 76%) of 3,4-difluorobenzoic acid, which can be obtained analytically pure from water (melting point 113°-120.5° C.).

후처리

  1. customto rise to 20° C
  2. additionwere then added
  3. extractionThe mixture was subsequently extracted twice with dichloromethane
  4. washthe organic phases were washed (NaHCO3) until the washings
  5. customThe solvent was then removed

출처 및 근거

ORD 기록
ord-3a540bda32044b3891e823049d0d41e1
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05481032

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