Formic Acid → 4-(3,4,5-Trifluorophenyl)cyclohexan-1-one

HRID 1769574노트

반응식

HRID 1769574 반응식
C(O)=O.C1(C)C=CC=CC=1.C1CO[C:13]2([CH2:18][CH2:17][CH:16]([C:19]3[CH:24]=[C:23]([F:25])[C:22]([F:26])=[C:21]([F:27])[CH:20]=3)[CH2:15][CH2:14]2)[O:12]1>O>[F:25][C:23]1[CH:24]=[C:19]([CH:16]2[CH2:15][CH2:14][C:13](=[O:12])[CH2:18][CH2:17]2)[CH:20]=[C:21]([F:27])[C:22]=1[F:26]

참가 물질

5

반응물 3

HCID 284Formic AcidHCID 1140TolueneHCID 867484001,1-Ethylenedioxy4-(3',4',5'-trifluorophenyl)-cyclohexane

생성물 1

HCID 219932844-(3,4,5-Trifluorophenyl)cyclohexan-1-one수율 79.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Formic acid (82.7 g) and toluene (20 ml) were added to 1,1-ethylenedioxy-4-(3',4', 5'-trifluorophenyl)cyclohexane (95.02 g), followed by heating the mixture under reflux with stirring for 2 hours, adding the reaction solution to water (500 ml), extracting with ethyl acetate (1 l), drying the organic layer over anhydrous magnesium sulfate, distilling off the solvent under reduced pressure, and recrystallizing from ethanol, to obtain 4-(3',4',5'-trifluorophenyl)cyclohexanone (63.1 g). m.p. 123.5° C.

후처리

  1. temperatureby heating the mixture
  2. temperatureunder reflux
  3. extractionextracting with ethyl acetate (1 l)
  4. dry with materialdrying the organic layer over anhydrous magnesium sulfate
  5. distillationdistilling off the solvent under reduced pressure
  6. customrecrystallizing from ethanol

출처 및 근거

ORD 기록
ord-bf938f53a585426caee9bf0f3e47c307
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05382379

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