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

HRID 1769572노트

반응식

HRID 1769572 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-8f6ba38ba29a4fe4bcefc74f2c52acff
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05382379

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