Phosphorus pentachloride → 1-Benzothiophene-3-sulfonyl chloride

HRID 1060533

반응식

HRID 1060533 반응식
[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]

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 86584280HCID 86584280, 화합물

생성물 1

HCID 27763401-Benzothiophene-3-sulfonyl chloride

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매2회

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-41e29d6c022745e5bea0d71adff2c06d
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525045B2

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