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

HRID 580442

反応式

HRID 580442 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-59b20f115b044d7f98e09f2d562d88f8
出典データセット
uspto-grants-1988_06
特許番号
US04753925

関連ノート

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