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Sodium Hydroxide → 3-(2-Bromo-5-(trifluoromethyl)phenyl)propanoic acid

HRID 1191922
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반응식

HRID 1191922 반응식
C([O:3][C:4](=[O:23])[CH:5]([CH2:11][C:12]1[CH:17]=[C:16]([C:18]([F:21])([F:20])[F:19])[CH:15]=[CH:14][C:13]=1[Br:22])C(OCC)=O)C.[OH-].[Na+]>C(O)C.O>[Br:22][C:13]1[CH:14]=[CH:15][C:16]([C:18]([F:21])([F:20])[F:19])=[CH:17][C:12]=1[CH2:11][CH2:5][C:4]([OH:23])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 53704455Diethyl [2-bromo-5-(trifluoromethyl)benzyl]malonate

생성물 1

HCID 248204723-(2-Bromo-5-(trifluoromethyl)phenyl)propanoic acid

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

To a solution of diethyl[2-bromo-5-(trifluoromethyl)benzyl]malonate (22.9 g, 57.6 mmol) in ethanol (100 mL) and water (50 mL) was added a 5 M solution of sodium hydroxide in water (30 mL). The mixture was heated to reflux for 2 h. Ethanol was removed by evaporation. The aqueous layer was extracted with ether and then acidified with concentrated HCl to pH 5 at which time a lot of white solid precipitated out. The solid was collected by filtration. The filtrate was extracted with ethyl acetate twice, and the extracts were washed with brine, dried (MgSO4) and concentrated to give a white solid.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 2 h
  3. customEthanol was removed by evaporation
  4. extractionThe aqueous layer was extracted with ether
  5. customprecipitated out
  6. filtrationThe solid was collected by filtration
  7. extractionThe filtrate was extracted with ethyl acetate twice
  8. washthe extracts were washed with brine
  9. dry with materialdried (MgSO4)
  10. concentrationconcentrated
  11. customto give a white solid

출처 및 근거

ORD 기록
ord-7a1b2f0395e5423d8a0cd82daf0a7c63
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08680104B2

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