p-Toluenesulfonic acid monohydrate → 1,1-Ethylenedioxy-4-(3,4',5'-trifluorophenyl)-3-cyclohexen

HRID 1769572ノート

反応式

HRID 1769572 の反応式
[CH2:1]1[CH2:20][O:19][C:3]2([CH2:8][CH2:7][C:6](O)([C:9]3[CH:14]=[C:13]([F:15])[C:12]([F:16])=[C:11]([F:17])[CH:10]=3)[CH2:5][CH2:4]2)[O:2]1.CC1C=CC(S(O)(=O)=O)=CC=1.O>C1(C)C=CC=CC=1>[CH2:20]1[CH2:1][O:2][C:3]2([CH2:8][CH2:7][C:6]([C:9]3[CH:14]=[C:13]([F:15])[C:12]([F:16])=[C:11]([F:17])[CH:10]=3)=[CH:5][CH2:4]2)[O:19]1

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 867483998-(3,4,5-Trifluorophenyl)-1,4-dioxaspiro[4.5]decan-8-ol

生成物 1

HCID 572149021,1-Ethylenedioxy-4-(3,4',5'-trifluorophenyl)-3-cyclohexen収率 65.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1,1-Ethylenedioxy-4-hydroxy-4-(3',4',5'-trifluoro-phenyl)cyclohexane (166.2 g) was dissolved in toluene (500 ml), followed by adding p-toluenesulfonic acidmonohydrate (20 g) into the solution, stirring the mixture under reflux for one hour, washing the reaction solution with water (500 ml), drying the organic layer over anhydrous magnesium sulfate, and distilling off the solvent under reduced pressure, to obtain 1,1-ethylenedioxy-4-(3',4',5'-trifluorophenyl)-3-cyclohexene (102.6 g).

後処理

  1. temperatureunder reflux for one hour
  2. washwashing the reaction solution with water (500 ml)
  3. dry with materialdrying the organic layer over anhydrous magnesium sulfate
  4. distillationdistilling off the solvent under reduced pressure

出典と根拠

ORDレコード
ord-8f6ba38ba29a4fe4bcefc74f2c52acff
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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