Water → HCID 22273264, Verbindung

HRID 1064357Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1064357
[Cl:1][C:2]1[C:8](Cl)=[CH:7][C:5]([NH2:6])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.[NH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.C(=O)([O-])[O-].[Na+].[Na+].O>C1(O)CCCCC1>[Cl:1][C:2]1[C:8]([N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)=[CH:7][C:5]([NH2:6])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 4837PiperazineHCID 10340Sodium CarbonateHCID 811494,5-Dichloro-2-nitroaniline

Produkt 1

HCID 22273264HCID 22273264, VerbindungAusbeute 84,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7966CyclohexanolLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

Into a solution of 20.02 g of 4,5-dichloro-2-nitroaniline and 8.70 g of piperazine in 100 ml of cyclohexanol, 12.80 g of sodium carbonate was added and stirred at 150° C. for 14 hours. Cooling the reaction liquid to room temperature, water was added and the system was extracted with chloroform. The chloroform layer was dried on anhydrous magnesium sulfate and the solvent was distilled off. Thus obtained residue was washed with diisopropyl ether to provide 21.07 g of 4-chloro-2-nitro-5-(piperazin-1-yl) aniline as a yellow powder.

Aufarbeitung

  1. temperatureCooling
  2. customthe reaction liquid to room temperature
  3. extractionthe system was extracted with chloroform
  4. dry with materialThe chloroform layer was dried on anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off
  6. washThus obtained residue was washed with diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-bc7791d27df84f43bfad8bc268e4517b
Quelldatensatz
uspto-grants-2005_11
Patentnummer
US06969712B2

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