2-Phenylthiophene → 2-Phenyl-5-(phenylthio)thiophene

HRID 46643

反応式

HRID 46643 の反応式
[C:1]1([C:7]2[S:8][CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:12]1([S:18]Cl)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>[Fe].C(Cl)(Cl)(Cl)Cl>[C:1]1([C:7]2[S:8][C:9]([S:18][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[CH:10][CH:11]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 2

HCID 699992-PhenylthiopheneHCID 11008040Benzenesulfenyl chloride

生成物 1

HCID 203867042-Phenyl-5-(phenylthio)thiophene収率 17.2%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 5943Carbon Tetrachloride溶媒

実験手順

In a 500 ml flask were placed 36.9 g (0.23 mole) of 2-phenylthiophene, 200 ml of reagent carbon tetrachloride, 36.9 g (0.26 mole) of benzenesulfenyl chloride and 0.2 g of iron powder. The reaction mixture was allowed to stand four days at room temperature. Distillation of the carbon tetrachloride gave a crystalline residue which was recrystallized first from ethanol-ethyl acetate (9:1) and then from ethyl acetate-pentane (1:9) to give 10.6 g (17%) of 2-phenyl-5-(phenylthio)thiophene, m.p. 72.5°-74.5° C.

後処理

  1. customIn a 500 ml flask were placed
  2. distillationDistillation of the carbon tetrachloride
  3. customgave a crystalline residue which
  4. customwas recrystallized first from ethanol-ethyl acetate (9:1)

出典と根拠

ORDレコード
ord-f02972133e9b4fe0a5e9eac8f921a27f
出典データセット
uspto-grants-1979_11
特許番号
US04174405

関連ノート

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