p-Toluenesulfonic acid → Ethyl 2-chloro-3,5-difluoro-4-methylbenzoyl-acetate

HRID 34574노트

반응식

HRID 34574 반응식
C1(C)C=CC(S(O)(=O)=O)=CC=1.[Cl:12][C:13]1[C:31]([F:32])=[C:30]([CH3:33])[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>[Cl:12][C:13]1[C:31]([F:32])=[C:30]([CH3:33])[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]

참가 물질

4

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 13657389Diethyl 2-chloro-3,5-difluoro-4-methylbenzoyl-malonate

생성물 1

HCID 13657390Ethyl 2-chloro-3,5-difluoro-4-methylbenzoyl-acetate수율 63.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

0.1 g of p-toluenesulphonic acid is added to an emulsion of 65.1 g of crude diethyl 2-chloro-3,5-difluoro-4-methyl-benzoyl-malonate in 70 ml of water. The mixture is heated to the boiling point for 4.5 hours, with thorough stirring, the cooled 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 under a fine vacuum gives 33 g of ethyl 2-chloro-3,5-difluoro-4-methylbenzoyl-acetate of boiling point 108°-118° C./0.09 mbar.

후처리

  1. temperatureThe mixture is heated to the boiling point for 4.5 hours, with thorough stirring
  2. extractionthe cooled 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

출처 및 근거

ORD 기록
ord-0f67ad4cd38d4a54b3752986c0a4cebc
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04762844

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