p-Toluenesulfonic acid monohydrate → 1,1'-(Prop-1-ene-1,1-diyl)bis(4-fluorobenzene)

HRID 1282471ノート

反応式

HRID 1282471 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)(O)[CH2:9][CH3:10])=[CH:4][CH:3]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([C:12]2[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=2)=[CH:9][CH3:10])=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 18424484HCID 18424484、化合物

生成物 1

HCID 184244971,1'-(Prop-1-ene-1,1-diyl)bis(4-fluorobenzene)収率 92%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

Into a reactor were introduced 2.80 g (11.3 mmol) of the 1,1-bis(4-fluorophenyl)propanol, 60 mL of toluene, and 14 mg of p-toluenesulfonic acid monohydrate under a nitrogen atmosphere. Azeotropic dehydration was conducted for 1 hour with toluene refluxing. After being cooled, the reaction mixture was washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution, subsequently dried with anhydrous magnesium sulfate, and then concentrated under reduced pressure to obtain 2.39 g (92%) of the target compound as white crystals.

後処理

  1. temperatureAfter being cooled
  2. washthe reaction mixture was washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution
  3. dry with materialsubsequently dried with anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-59803f55663c495981c236257284bf15
出典データセット
uspto-grants-2002_09
特許番号
US06455720B1

反応ノート

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