Sodium Hydroxide → 2-(3,4-Dimethoxyphenyl)-4-(trifluoromethyl)benzoic acid

HRID 439546노트

반응식

HRID 439546 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[CH:18][C:12]=2[C:13]([O:15]CC)=[O:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[OH-].[Na+]>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[CH:21]=[C:20]([C:22]([F:23])([F:25])[F:24])[CH:19]=[CH:18][C:12]=2[C:13]([OH:15])=[O:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 15766263Ethyl 2-(3,4-dimethoxyphenyl)-4-(trifluoromethyl)benzoate

생성물 1

HCID 157662622-(3,4-Dimethoxyphenyl)-4-(trifluoromethyl)benzoic acid수율 90%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1000 ml of absolute ethanol, 290 g (0.82 mol) of ethyl 2-(3,4-dimethoxyphenyl)-4-(trifluoromethyl)benzoate and 170 ml (0.164 mol) of 10N sodium hydroxide solution are introduced successively into a 2-liter round-bottomed flask. The reaction mixture is brought to reflux for two hours and then evaporated to dryness under reduced pressure. The residue is taken up in 2.5 liters of water and extracted successively with 500 ml of ethyl acetate and 500 ml of pentane. 500 g of crushed ice are added to the aqueous phase which is then treated with an excess of concentrated hydrochloric acid. The precipitate which forms is filtered on sintered glass and then dried under a stream of air; there is thus obtained 240.5 g (yield: 90%) of 2-(3,4-dimethoxyphenyl)-4-(trifluoromethyl)benzoic acid in the form of a light-beige solid melting at 194° C.

후처리

  1. temperatureto reflux for two hours
  2. customevaporated to dryness under reduced pressure
  3. extractionextracted successively with 500 ml of ethyl acetate and 500 ml of pentane
  4. addition500 g of crushed ice are added to the aqueous phase which
  5. additionis then treated with an excess of concentrated hydrochloric acid
  6. filtrationThe precipitate which forms is filtered on sintered glass
  7. customdried under a stream of air

출처 및 근거

ORD 기록
ord-726e33990802421f97e6c1525fe6182e
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05514719

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