Ethyl Acetate → 2,4,5-Trifluoro-3-methoxybenzoic acid

HRID 358876

반응식

HRID 358876 반응식
[OH-].[Na+].[CH3:3][O:4][C:5]1[C:6]([F:16])=[C:7]([CH:11]=[C:12]([F:15])[C:13]=1[F:14])[C:8](N)=[O:9].C(OCC)(=[O:19])C>O>[CH3:3][O:4][C:5]1[C:6]([F:16])=[C:7]([CH:11]=[C:12]([F:15])[C:13]=1[F:14])[C:8]([OH:19])=[O:9]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 27752782,4,5-Trifluoro-3-methoxybenzamide

생성물 1

HCID 27339702,4,5-Trifluoro-3-methoxybenzoic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

226 ml (0.226 mole) of a 1N aqueous solution of sodium hydroxide were added to a suspension of 46.4 g (0.226 mole) of 3-methoxy-2,4,5-trifluorobenzamide (XXV) [prepared as described in Step (E5) above] in 900 ml of water, and the mixture was heated under reflux with stirring for 2 hours. At the end of this time, the reaction mixture was cooled to room temperature and then shaken with ethyl acetate to remove unreacted material. The aqueous layer was separated and acidified with hydrochloric acid to precipitate a crystalline substance, which was extracted with ethyl acetate. The extract was washed with water and dried, and the solvent was removed by evaporation under reduced pressure to afford 37.1 g of 3-methoxy-2,4,5-trifluorobenzoic acid (XXVI) as colorless needles having the same properties as the product of Preparation 1.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. customto remove unreacted material
  4. customThe aqueous layer was separated
  5. customto precipitate a crystalline substance, which
  6. extractionwas extracted with ethyl acetate
  7. washThe extract was washed with water
  8. customdried
  9. customthe solvent was removed by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-6926643e649244f09054354f2addc780
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997943

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