Hydrochloric Acid → HCID 53652618, Verbindung

HRID 128256

Reaktionsgleichung

[Na+].[C:2]([C:5]1[S:9][C:8]2[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=2[C:6]=1[S:14]([O-:17])(=O)=[O:15])(O)=[O:3].P(Cl)(Cl)(Cl)(Cl)[Cl:19].[ClH:24]>P(Cl)(Cl)(Cl)=O>[Cl:24][C:2]([C:5]1[S:9][C:8]2[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=2[C:6]=1[S:14]([Cl:19])(=[O:17])=[O:15])=[O:3]

Komponenten

Reaktionsbedingungen

Temperatur: 100 °C

Versuchsvorschrift

44.0 gm (0.157 mol) of the above 2-carboxy-benzo[b]thiophene-3-sulfonic acid mono sodium salt were suspended in 200 cc of phosphorus oxychloride and admixed with 65.4 gm (0.314 mol) of phosphorus-(V)-chloride. To complete the reaction which was exothermic in the beginning accompanied by evolution of hydrogen chloride, the reaction mixture was heated to 100° C. for 2 hours, cooled and the inorganic salts were filtered off. After evaporation in vacuo, the residue was taken up in 300 cc of dry chloroform, the solution was filtered and again evaporated. The oily residue, consisting of 27 gm (58% of theory) of raw 2-chlorocarbonyl-benzo[b]thiophene-3-sulfonic acid chloride, crystallized upon cooling (m.p. 45°-47° C.) and was used without further purification in the next step.

Aufarbeitung

customthe reaction which
temperaturecooled
filtrationthe inorganic salts were filtered off
customAfter evaporation in vacuo
filtrationthe solution was filtered
customagain evaporated
customcrystallized
temperatureupon cooling (m.p. 45°-47° C.)
customwas used without further purification in the next step

Quellen und Nachweise

ORD-Eintrag: ord-14d096795bba47acbafa6b123602e040
Quelldatensatz: uspto-grants-1981_03
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04259336

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