Ethanol → HCID 20183309, Verbindung

HRID 255731Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 255731
[CH3:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:3]=1[C:23]([NH2:25])=[O:24].C=O.[CH3:28][N:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1.[CH2:35](O)C>ClCCCl>[CH3:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:3]=1[C:23]([NH:25][CH2:28][N:29]1[CH2:34][CH2:33][N:32]([CH3:35])[CH2:31][CH2:30]1)=[O:24]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 712FormaldehydeHCID 531671-MethylpiperazineHCID 11724425HCID 11724425, Verbindung

Produkt 1

HCID 20183309HCID 20183309, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Versuchsvorschrift

A mixture of 6-methyl-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinecarboxamide (5 g), formalin (37%, 1.35 ml), N-methylpiperazine (2.25 g), ethanol (50 ml) and 1,2-dichloroethane (25 ml) was refluxed for 6 hours. After evaporating the solvent in vacuo, the residue was chromatographed on alumina (200 ml) and eluted with chloroform. The fractions containing the object compound were combined and concentrated under reduced pressure. The residue was recrystallized from diethyl ether to give 6-methyl-N-(4-methylpiperazin-1-ylmethyl)-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinecarboxamide (1.90 g).

Aufarbeitung

  1. temperaturewas refluxed for 6 hours
  2. customAfter evaporating the solvent in vacuo
  3. customthe residue was chromatographed on alumina (200 ml)
  4. washeluted with chloroform
  5. additionThe fractions containing the object compound
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was recrystallized from diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-002b837b81614d6783b6c08f9450c410
Quelldatensatz
uspto-grants-1987_10
Patentnummer
US04698340

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