Ethanol → HCID 23359031, Verbindung

HRID 2396961Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2396961
F[C:2]1[C:7]([F:8])=[C:6]([Cl:9])[C:5]([N+:10]([O-:12])=[O:11])=[C:4]([F:13])[C:3]=1[CH3:14].C(O)C.[CH3:18][N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1>O.C(N(CC)CC)C>[CH3:18][N:19]1[CH2:24][CH2:23][N:22]([C:2]2[C:7]([F:8])=[C:6]([Cl:9])[C:5]([N+:10]([O-:12])=[O:11])=[C:4]([F:13])[C:3]=2[CH3:14])[CH2:21][CH2:20]1

Komponenten

6

Edukt 3

HCID 702EthanolHCID 531671-MethylpiperazineHCID 23358995HCID 23358995, Verbindung

Produkt 1

HCID 23359031HCID 23359031, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

To 2,3,6-trifluoro-4-chloro-5-nitrotoluene (0.17 g) are added ethanol (3.3 ml), water (0.5 ml), N-methylpiperazine (0.45 ml) and triethylamine (0.56 ml) and the mixture is refluxed for 24 hours. After the reaction is completed, water is added to the reaction mixture and the mixture is extracted with diethyl ether, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and the residue is purified by silica-gel column-chromatography (eluent; dichloromethane: methanol=20 : 1) to give 2-(4-methyl-1-piperazinyl)-3,6-difluoro-4-chloro-5-nitrotoluene (0.13 g).

Aufarbeitung

  1. temperaturethe mixture is refluxed for 24 hours
  2. extractionthe mixture is extracted with diethyl ether
  3. washthe extract is washed with water
  4. customdried
  5. distillationThe solvent is distilled off under reduced pressure
  6. customthe residue is purified by silica-gel column-chromatography (eluent; dichloromethane: methanol=20 : 1)

Quellen und Nachweise

ORD-Eintrag
ord-40d4326fb4b54cc99073f5bb89638d1d
Quelldatensatz
uspto-grants-1996_02
Patentnummer
US05495020

Notizen zur Reaktion

Wird geladen…