Hydrochloric Acid → 2-Acetylphenoxathiin

HRID 1447558

Reaktionsgleichung

Reaktionsgleichung von HRID 1447558
[CH:1]1[C:14]2[S:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[O:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[C:15](Cl)(=[O:17])[CH3:16].[Cl-].[Al+3].[Cl-].[Cl-].Cl>C(=S)=S.O>[C:15]([C:10]1[CH:9]=[CH:8][C:7]2[O:6][C:5]3[C:14](=[CH:1][CH:2]=[CH:3][CH:4]=3)[S:13][C:12]=2[CH:11]=1)(=[O:17])[CH3:16]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 9217PhenoxathiinHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 5151742-Acetylphenoxathiin

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6348Carbon DisulfideLösungsmittel

Versuchsvorschrift

Phenoxathiin (22.9 g.) and acetyl chloride (8.8 ml) were dissolved in carbon disulphide (120 ml) and mechanically stirred while aluminium chloride (15.5 g) was added in small portions. The red mixture was stirred for 2 hr. at room temperature, then boiled under reflux on the water bath for a further 21/4 hr. The mixture was cooled and poured on to ice and hydrochloric acid, and the precipitated product filtered off, washed with water, and recrystallised once from ethanol and twice from petroleum ether (b.p. 80°-100° C.) to give the product m.p. 112° C.

Aufarbeitung

  1. additionwas added in small portions
  2. customat room temperature
  3. temperatureThe mixture was cooled
  4. filtrationthe precipitated product filtered off
  5. washwashed with water
  6. customrecrystallised once from ethanol and twice from petroleum ether (b.p. 80°-100° C.)

Quellen und Nachweise

ORD-Eintrag
ord-12af6377e2a04691b4736f8bc294de47
Quelldatensatz
uspto-grants-1979_12
Patentnummer
US04177257

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