p-Toluenesulfonic acid → Ethyl 3-oxo-(2,3,4,5-tetrafluorophenyl)propanoate

HRID 580442

반응식

HRID 580442 반응식
C1(C)C=CC(S(O)(=O)=O)=CC=1.[F:12][C:13]1[C:31]([F:32])=[C:30]([F:33])[C:29]([F:34])=[CH:28][C:14]=1[C:15]([CH:17](C(OCC)=O)[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[O:16]>O>[F:12][C:13]1[C:31]([F:32])=[C:30]([F:33])[C:29]([F:34])=[CH:28][C:14]=1[C:15]([CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])=[O:16]

참가 물질

4

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 135649731,3-Diethyl 2-(2,3,4,5-tetrafluorobenzoyl)propanedioate

생성물 1

HCID 600916Ethyl 3-oxo-(2,3,4,5-tetrafluorophenyl)propanoate수율 71.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

0.3 g of p-toluenesulphonic acid is added to an emulsion of 284.8 g of crude diethyl 2,3,4,5-tetrafluorobenzoyl-malonate in 300 ml of water. The mixture is heated at the boiling point for 4.5 hours, with thorough stirring, the cooled emulsion is extracted several times with methylene chloride, the combined methylene chloride solutions are washed once with saturated sodium chloride solution and dried with sodium sulphate and the solvent is distilled off in vacuo. Fractionation of the residue under a fine vacuum gives 160.2 g of ethyl 2,3,4,5-tetrafluorobenzoylacetate of boiling point 75°-96° C./0.06-0.09 mbar.

후처리

  1. temperatureThe mixture is heated at the boiling point for 4.5 hours, with thorough stirring
  2. extractionthe cooled emulsion is extracted several times with methylene chloride
  3. washthe combined methylene chloride solutions are washed once with saturated sodium chloride solution
  4. dry with materialdried with sodium sulphate
  5. distillationthe solvent is distilled off in vacuo

출처 및 근거

ORD 기록
ord-59b20f115b044d7f98e09f2d562d88f8
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04753925

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