Acetic Acid → 2-Methoxy-4-trifluoromethanesulfonyloxybenzoic acid

HRID 2243521노트

반응식

HRID 2243521 반응식
[CH3:1][O:2][C:3]1[CH:12]=[C:11]([O:13][S:14]([C:17]([F:20])([F:19])[F:18])(=[O:16])=[O:15])[CH:10]=[CH:9][C:4]=1[C:5]([O:7]C)=[O:6].S(=O)(=O)(O)O.C(O)(=O)C>O>[CH3:1][O:2][C:3]1[CH:12]=[C:11]([O:13][S:14]([C:17]([F:20])([F:18])[F:19])(=[O:16])=[O:15])[CH:10]=[CH:9][C:4]=1[C:5]([OH:7])=[O:6]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 23282575Methyl 2-methoxy-4-trifluoromethane-sulfonyloxybenzoate

생성물 1

HCID 231343522-Methoxy-4-trifluoromethanesulfonyloxybenzoic acid수율 37.5%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A mixture of methyl 2-methoxy-4-trifluoromethane-sulfonyloxybenzoate (3.49 g), sulfuric acid (90%, 0.1 mL), acetic acid (10 mL) and water (2 mL) was heated under reflux for 16 hrs. The reaction mixture was diluted with water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over an hydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by recrystallization (solvent: ethyl acetate/n-hexane) to afford the title compound (1.25 g).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hrs
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over an hydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe residue was purified by recrystallization (solvent: ethyl acetate/n-hexane)

출처 및 근거

ORD 기록
ord-aafc8c027b5b4da2b53de7266f47d3f5
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07674938B2

반응 노트

불러오는 중…