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

HRID 974938

반응식

HRID 974938 반응식
[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]

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

0.04 g of p-toluenetoluenesulphonic acid is added to an emulsion of 34.7 g of crude diethyl (2,4-di-chloro-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.

후처리

  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

출처 및 근거

ORD 기록
ord-166092886df9427db7977325063c8730
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05607942

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