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Sodium Hydroxide → 2,6-dichloro-4-(trifluoromethyl)benzoic Acid

HRID 342972
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HRID 342972 반응식
[OH-].[Na+].[Cl:3][C:4]1[CH:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=[C:11]([Cl:19])[C:5]=1[C:6]([O:8]CC)=[O:7]>O.C(O)C>[Cl:3][C:4]1[CH:14]=[C:13]([C:15]([F:16])([F:17])[F:18])[CH:12]=[C:11]([Cl:19])[C:5]=1[C:6]([OH:8])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 54315306Ethyl 2,6-dichloro-4-(trifluoromethyl)benzoate

생성물 1

HCID 116804602,6-dichloro-4-(trifluoromethyl)benzoic Acid수율 71.7%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of sodium hydroxide (41.6 g) in water was added to a solution of ethyl 2,6-dichloro-4-trifluoromethylbenzoate (96.3 g) in ethanol. The mixture was heated at reflux for 2.5 hours then cooled and evaporated. It was diluted with water and extracted with ether. The aqueous layer was acidified to pH1 and extracted with ether, washed with water, dried (Na2SO4) and filtered. The filtrate was evaporated to dryness and the residue was triturated with n-hexane and filtered to give 2.6-dichloro-4-trifluoromethylbenzoic acid (62.3 g) as a white solid mp 138.5°-139° C.

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후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 2.5 hours
  3. temperaturethen cooled
  4. customevaporated
  5. additionIt was diluted with water
  6. extractionextracted with ether
  7. extractionextracted with ether
  8. washwashed with water
  9. dry with materialdried (Na2SO4)
  10. filtrationfiltered
  11. customThe filtrate was evaporated to dryness
  12. customthe residue was triturated with n-hexane
  13. filtrationfiltered

출처 및 근거

ORD 기록
ord-616c99d8fc034996bc893d6f2e593ffa
출처 데이터셋
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05859283

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