Sodium Hydroxide → 2,6-Difluoro-3,5-dimethoxybenzoic acid

HRID 459943노트

반응식

HRID 459943 반응식
C[O:2][C:3](=[O:16])[C:4]1[C:9]([F:10])=[C:8]([O:11][CH3:12])[CH:7]=[C:6]([O:13][CH3:14])[C:5]=1[F:15].[OH-].[Na+]>C(O)C>[F:10][C:9]1[C:8]([O:11][CH3:12])=[CH:7][C:6]([O:13][CH3:14])=[C:5]([F:15])[C:4]=1[C:3]([OH:16])=[O:2]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 59486229Methyl 2,6-difluoro-3,5-dimethoxybenzoate

생성물 1

HCID 184447022,6-Difluoro-3,5-dimethoxybenzoic acid수율 82.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A suspension of 115 g (0.49 mol) of 2,6-difluoro-3,5-dimethoxy benzoic acid methyl ester and 42.9 g (1.07 mol) of solid sodium hydroxide in 1.4 L of anhydrous ethanol was refluxed for 24 hours. The ethanol was concentrated in vacuo and the solid residue was dissolved in water and extracted two times with ethyl ether. The aqueous layer was acidified with concentrated hydrochloric acid and a white precipitate was filtered, washed with cold water and dried in vacuo to give 87.9 g (81%) of the title compound. MS (APCI) (m+1)/z 219.1.

후처리

  1. temperaturewas refluxed for 24 hours
  2. concentrationThe ethanol was concentrated in vacuo
  3. dissolutionthe solid residue was dissolved in water
  4. extractionextracted two times with ethyl ether
  5. filtrationa white precipitate was filtered
  6. washwashed with cold water
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-f2d00457297a4452b22bed72baeea1e4
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07196090B2

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