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Ethanol → Ethyl 3-(2,4-difluorophenyl)prop-2-enoate

HRID 612946
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HRID 612946 반응식
[F:1][C:2]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:3]=1[CH:4]=[CH:5][C:6]([OH:8])=[O:7].S(=O)(=O)(O)O.[CH2:19](O)[CH3:20]>>[CH2:19]([O:7][C:6](=[O:8])[CH:5]=[CH:4][C:3]1[CH:9]=[CH:10][C:11]([F:13])=[CH:12][C:2]=1[F:1])[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 6035023-(2,4-Difluorophenyl)acrylic Acid

생성물 1

HCID 53395691Ethyl 3-(2,4-difluorophenyl)prop-2-enoate수율 97%

실험 절차

2,4-Difluorocinnamic acid (10.1 g) was dissolved in ethanol (100 ml), and conc. sulfuric acid (1 ml) was added thereto, and the resulting mixture was refluxed for 3 hours. The solvent was evaporated under reduced pressure and the residue was poured into ice-cold water and extracted with ethyl acetate. The extract was washed successively with 5% aqueous sodium hydrogencarbonate and a saturated aqueous NaCl solution, and the organic layer was dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure to obtain the title compound (11.2 g, 97%) as a colorless oil.

후처리

  1. temperaturethe resulting mixture was refluxed for 3 hours
  2. customThe solvent was evaporated under reduced pressure
  3. additionthe residue was poured into ice-cold water
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed successively with 5% aqueous sodium hydrogencarbonate
  6. dry with materiala saturated aqueous NaCl solution, and the organic layer was dried over anhydrous magnesium sulfate
  7. filtrationAfter filtration
  8. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-edcfeb9509c1427793abc0199299ed2d
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06005116

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