Phosphorus pentachloride → 2-(4-Chloro-phenylsulfonylamino)4,5-dimethoxy-benzoyl chloride

HRID 425749Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 425749
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[CH:17][C:13]=2[C:14](O)=[O:15])(=[O:10])=[O:9])=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:26]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[CH:17][C:13]=2[C:14]([Cl:26])=[O:15])(=[O:10])=[O:9])=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 24819Phosphorus pentachlorideHCID 12399912-{[(4-Chlorophenyl)sulfonyl]amino}-4,5-dimethoxybenzoic acid

Produkt 1

HCID 98433672-(4-Chloro-phenylsulfonylamino)4,5-dimethoxy-benzoyl chlorideAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
42.5 °C

Versuchsvorschrift

25.90 g (0.07 mol) of 2-(4-chloro-phenylsulfonylamino)-4,5-dimethoxy-benzoic acid were mixed with 75 ml of toluene, 17.30 g (0.08 mol) of phosphorus pentachloride were added and the mixture was stirred at 40-45° C. for 2.5 h. Then the mixture was concentrated in vacuo to half of its volume and the product that precipitated was filtered off with suction and washed with a small amount of toluene. 25.30 g (93%) of 2-(4-chloro-phenylsulfonylamino)-4,5-dimethoxy-benzoyl chloride having a melting point of 175-177° C. were obtained.

Aufarbeitung

  1. additionwere added
  2. concentrationThen the mixture was concentrated in vacuo to half of its volume
  3. customthe product that precipitated
  4. filtrationwas filtered off with suction
  5. washwashed with a small amount of toluene

Quellen und Nachweise

ORD-Eintrag
ord-17f0651b37a440758c4ad635bf1ae911
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08106213B2

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