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Toluene → 1-Ethoxy-2,3-difluoro-4-(4-(3-propylcyclopentyl)cyclohex-1-enyl)benzene

HRID 1464848
ノート
印刷プレビュー

反応式

HRID 1464848 の反応式
C1(C)C=CC=CC=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:20]([O:22][C:23]1[CH:28]=[CH:27][C:26]([C:29]2(O)[CH2:34][CH2:33][CH:32]([CH:35]3[CH2:39][CH2:38][CH:37]([CH2:40][CH2:41][CH3:42])[CH2:36]3)[CH2:31][CH2:30]2)=[C:25]([F:44])[C:24]=1[F:45])[CH3:21]>O>[CH2:20]([O:22][C:23]1[CH:28]=[CH:27][C:26]([C:29]2[CH2:34][CH2:33][CH:32]([CH:35]3[CH2:39][CH2:38][CH:37]([CH2:40][CH2:41][CH3:42])[CH2:36]3)[CH2:31][CH:30]=2)=[C:25]([F:44])[C:24]=1[F:45])[CH3:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1140TolueneHCID 521998p-Toluenesulfonic acid monohydrateHCID 679923521-(4-Ethoxy-2,3-difluorophenyl)-4-(3-propylcyclopentyl)cyclohexanol

生成物 1

HCID 679922881-Ethoxy-2,3-difluoro-4-(4-(3-propylcyclopentyl)cyclohex-1-enyl)benzene収率 82%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Toluene (50 ml) and p-toluenesulfonic acid monohydrate (0.15 g) were added to 1-(4-ethoxy-2,3-difluorophenyl)-4-(3-propylcyclopentyl)cyclohexanol (5.0 g) obtained in the first step, in a reaction vessel equipped with a Dean-Stark apparatus under an atmosphere of nitrogen. The mixture was refluxed for 1.5 hour, while forming water was removed with a Dean-Stark apparatus. After the mixture had been cooled to room temperature, the reaction solution was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (eluent: ethyl acetate/n-heptane=1/10 by volume) to give 1-ethoxy-2,3-difluoro-4-(4-(3-propylcyclopentyl)cyclohex-1-enyl)benzene (3.9 g).

後処理

  1. customobtained in the first step, in a reaction vessel
  2. customequipped with a Dean-Stark apparatus under an atmosphere of nitrogen
  3. temperatureThe mixture was refluxed for 1.5 hour
  4. customwas removed with a Dean-Stark apparatus
  5. washthe reaction solution was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure
  8. customThe residue was purified by silica gel chromatography (eluent: ethyl acetate/n-heptane=1/10 by volume)

出典と根拠

ORDレコード
ord-a0f318190e394d1f9a320580866fc285
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08999197B2

反応ノート

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