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

HRID 1769574ノート

反応式

HRID 1769574 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bf938f53a585426caee9bf0f3e47c307
出典データセット
uspto-grants-1995_01
特許番号
US05382379

反応ノート

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