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

HRID 36709

反応式

HRID 36709 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 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
  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-85d2a1a297be4b2a927b6c639d4588a1
出典データセット
uspto-grants-1995_05
特許番号
US05416096

関連ノート

読み込み中…