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

HRID 637288

反応式

HRID 637288 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 (3) in 300 ml of water. The mixture is heated to the boil for 5 hours, while stirring thoroughly, the cold emulsion is extracted several times with methylene chloride, the combined CH2CL2 solutions are washed once with saturated NaCl solution and dried with Na2SO4, and the solvent is distilled off in vacuo. Fractionation of the residue in a fine vacuum gives 160.2 g of ethyl 2,3,4,5-tetrafluorobenzoyl-acetate (4) of boiling point 100°-110° C./0.09-0.1 mbar. Melting point 47°-49° C.

後処理

  1. temperatureThe mixture is heated to the boil for 5 hours
  2. extractionthe cold emulsion is extracted several times with methylene chloride
  3. washthe combined CH2CL2 solutions are washed once with saturated NaCl solution
  4. dry with materialdried with Na2SO4
  5. distillationthe solvent is distilled off in vacuo

出典と根拠

ORDレコード
ord-fefb66db3584483abd71faf62b2df084
出典データセット
uspto-grants-1985_12
特許番号
US04556658

関連ノート

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