Phosphorus pentachloride → 1-Benzothiophene-3-sulfonyl chloride

HRID 1060533

反応式

HRID 1060533 の反応式
[Na].[S:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[C:4]([S:11]([O-:14])(=O)=[O:12])=[CH:3]1.P(Cl)(Cl)(Cl)(Cl)[Cl:16]>P(Cl)(Cl)(Cl)=O>[Cl:16][S:11]([C:4]1[C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[S:2][CH:3]=1)(=[O:14])=[O:12]

参加物

4

反応物 2

HCID 24819Phosphorus pentachlorideHCID 86584280HCID 86584280、化合物

生成物 1

HCID 27763401-Benzothiophene-3-sulfonyl chloride

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒2 回

実験手順

180 g of sodium-benzothiophene-3-sulphonate are placed in 650 ml of phosphorus oxychloride and then combined with 156 g of phosphorus pentachloride. The reaction mixture is refluxed for 3.5 hours before the excess phosphorus oxychloride is eliminated by distillation in vacuo. The residue is taken up in 800 ml of chloroform and the precipitate formed is separated off by filtering. The filtrate is concentrated by evaporation and stirred into 800 ml of petroleum ether with heating. The crystalline substance thus precipitated is filtered off, washed with petroleum ether and dried at 35° C.

後処理

  1. distillationis eliminated by distillation in vacuo
  2. customthe precipitate formed
  3. customis separated off
  4. filtrationby filtering
  5. concentrationThe filtrate is concentrated by evaporation
  6. temperaturewith heating
  7. customThe crystalline substance thus precipitated
  8. filtrationis filtered off
  9. washwashed with petroleum ether
  10. customdried at 35° C.

出典と根拠

ORDレコード
ord-41e29d6c022745e5bea0d71adff2c06d
出典データセット
uspto-grants-2003_02
特許番号
US06525045B2

関連ノート

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