Water → 2-Methoxy-4-(trifluoromethyl)benzoic acid

HRID 1181425

반응식

HRID 1181425 반응식
[CH3:1][O:2][C:3]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:4]=1[C:5]#N.[OH-:15].[K+].[OH2:17]>C(O)C>[CH3:1][O:2][C:3]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:4]=1[C:5]([OH:17])=[O:15]

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 190013762-Methoxy-4-(trifluoromethyl)benzonitrile

생성물 1

HCID 36908732-Methoxy-4-(trifluoromethyl)benzoic acid수율 95%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 2-methoxy-4-(trifluoromethyl)benzonitrile (Description 94; 19 g, 94.4 mmol) in ethanol (150 ml) was added a solution of potassium hydroxide (26.43 g; 472 mmol) in water (100 ml) and the resulting mixture heated at reflux overnight. The mixture was cooled and the ethanol removed by evaporation, the remaining aqueous phase was extracted with diethyl ether then acidified with 5N HCl. The acidic aqueous phase was then extracted with EtOAc (3×200 ml) and the combined organic layers washed with water, sat NaCl, dried over Na2SO4, filtered and evaporated to give the title compound (19.91 g, 95%).

후처리

  1. temperaturethe resulting mixture heated
  2. temperatureat reflux overnight
  3. temperatureThe mixture was cooled
  4. customthe ethanol removed by evaporation
  5. extractionthe remaining aqueous phase was extracted with diethyl ether
  6. extractionThe acidic aqueous phase was then extracted with EtOAc (3×200 ml)
  7. washthe combined organic layers washed with water
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. customevaporated

출처 및 근거

ORD 기록
ord-e989d54aadff4961beaccc9c62ce0d01
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07285563B2

연결된 노트

불러오는 중…