Diethyl (2,4-dichloro-3,6-difluorobenzoyl)-malonate → Ethyl (2,4-dichloro-3,6-difluorobenzoyl)acetate

HRID 345843

反応式

HRID 345843 の反応式
[Cl:1][C:2]1[C:20]([F:21])=[C:19]([Cl:22])[CH:18]=[C:17]([F:23])[C:3]=1[C:4]([CH:6](C(OCC)=O)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]>O>[Cl:1][C:2]1[C:20]([F:21])=[C:19]([Cl:22])[CH:18]=[C:17]([F:23])[C:3]=1[C:4]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]

参加物

3

反応物 1

HCID 15070034Diethyl (2,4-dichloro-3,6-difluorobenzoyl)-malonate

生成物 1

HCID 15070035Ethyl (2,4-dichloro-3,6-difluorobenzoyl)acetate収率 49.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

0.04 g of p-toluenetoluenesulphonic acid is added to an emulsion of 34.7 g of crude diethyl (2,4-dichloro-3,6-difluorobenzoyl)-malonate in 40 ml of water. The mixture is heated at the boiling point for 3 hours, while stirring thoroughly, the cooled emulsion is extracted several times with methylene chloride, the combined CH2Cl2 solutions are washed once with saturated sodium chloride solution and PG,130 dried with Na2SO4 and the solvent is distilled off in vacuo. Fractionation of the residue (33.9 g) in vacuo gives 13.9 g of ethyl (2,4-dichloro-3,6-difluorobenzoyl)-acetate of boiling point 110°-115° C./0.05 mbar, nD25 : 1,5241.

後処理

  1. temperatureThe mixture is heated at the boiling point for 3 hours
  2. extractionthe cooled emulsion is extracted several times with methylene chloride
  3. washthe combined CH2Cl2 solutions are washed once with saturated sodium chloride solution and PG,130
  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-0f89583892b446bfab9a349834faac80
出典データセット
uspto-grants-1991_10
特許番号
US05059597

関連ノート

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