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

HRID 280100

반응식

HRID 280100 반응식
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]

참가 물질

4

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 135649731,3-Diethyl 2-(2,3,4,5-tetrafluorobenzoyl)propanedioate

생성물 1

HCID 600916Ethyl 3-oxo-(2,3,4,5-tetrafluorophenyl)propanoate수율 71.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

0.3 g of p-toluenesulphonic acid is added to an emulsion of 284.8 g of crude diethyl 2,3,4,5-tetrafluorobenzoylmalonate in 300 ml of water. The emulsion is heated to boiling for 5 hours, stirring vigorously, then it is cooled and extracted several times with methylene chloride, and the combined methylene chloride solutions are washed once with saturated NaCl solution, dried with Na2SO4, and the solvent is removed by distillation in vacuo. Fractionation of the residue under fine vacuum provides 160.2 g of ethyl 2,3,4,5-tetrafluorobenzoylacetate of boiling point 100°-110° C./0.09-0.1 mbar. Melting point 47°-49° C.

후처리

  1. temperatureThe emulsion is heated
  2. temperatureit is cooled
  3. extractionextracted several times with methylene chloride
  4. washthe combined methylene chloride solutions are washed once with saturated NaCl solution
  5. dry with materialdried with Na2SO4
  6. customthe solvent is removed by distillation in vacuo

출처 및 근거

ORD 기록
ord-eae4ea0c172548a29248d522207cf253
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04588726

연결된 노트

불러오는 중…