Sodium Carbonate → HCID 21697868, Verbindung

HRID 379082

Reaktionsgleichung

Reaktionsgleichung von HRID 379082
C(=O)([O-])[O-].[Na+].[Na+].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([N+:14]([O-:16])=[O:15])[C:9]=1Cl.[Cl:18][C:19]1[CH:24]=[C:23]([Cl:25])[CH:22]=[CH:21][C:20]=1[SH:26]>C1(C)C(C)=CC=CC=1>[Cl:7][C:8]1[C:9]([S:26][C:20]2[CH:21]=[CH:22][C:23]([Cl:25])=[CH:24][C:19]=2[Cl:18])=[C:10]([N+:14]([O-:16])=[O:15])[CH:11]=[CH:12][CH:13]=1

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 185552,3-DichloronitrobenzeneHCID 707302,4-Dichlorobenzenethiol

Produkt 1

HCID 21697868HCID 21697868, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

Sodium carbonate (13.8 g) is added to a solution of 1,2-dichloro-3-nitrobenzene (19.29 g) and 2,4-dichlorothio-phenol (17.9 g) in xylene (250 ml), and the resulting mixture is heated for 5 hours at reflux temperature. The precipitate is separated by filtration, washed with xylene and the combined organic phases are concentrated. The resultant residue is mixed with petroleum ether and stirred for 1 hour at room temperature. Following this, the crystalline material is suction filtered and washed with petroleum ether, and any remaining solvent is removed in a vacuum. Yield: 25.6 g of colourless crystals (76.6%).

Aufarbeitung

  1. temperaturethe resulting mixture is heated for 5 hours
  2. temperatureat reflux temperature
  3. customThe precipitate is separated by filtration
  4. washwashed with xylene
  5. concentrationthe combined organic phases are concentrated
  6. additionThe resultant residue is mixed with petroleum ether
  7. filtrationfiltered
  8. washwashed with petroleum ether
  9. customany remaining solvent is removed in a vacuum

Quellen und Nachweise

ORD-Eintrag
ord-2fb5417e2cc842c6ac1694a12d2490dc
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06297282B1

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