Thionyl Chloride → HCID 19804733, Verbindung

HRID 1709339Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1709339
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].S(Cl)([Cl:17])=O>>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[CH:8]=[CH:7][C:3]=1[C:4]([Cl:17])=[O:5]

Komponenten

3

Versuchsvorschrift

23.0 g of 2,4-dichloro-3-nitrobenzoic acid and 150 ml of thionyl chloride were refluxed for 6 hours under heating. Then, thionyl chloride was distilled off to obtain crude 2,4-dichloro-3-nitrobenzoyl chloride. 200 ml of methanol was added to the crude compound and refluxed under heating. Methanol was distilled off, and then ethyl acetate was added thereto to obtain an ethyl acetate solution. The solution was washed sequentially with a 5% sodium hydroxide aqueous solution, diluted hydrochloric acid and water. After drying, the solvent was distilled off to obtain 21.8 g of the desired product. Melting point: 72°-74° C.

Aufarbeitung

  1. temperatureunder heating
  2. distillationThen, thionyl chloride was distilled off

Quellen und Nachweise

ORD-Eintrag
ord-a76fa3f85f0649659f286e690fb7fb7c
Quelldatensatz
uspto-grants-1990_08
Patentnummer
US04948887

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