1-(m-Tolyl)piperazine → HCID 12414812, Verbindung

HRID 1657409Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1657409
Cl[CH2:2][CH2:3][C:4]1[C:9](=[O:10])[N:8]2[CH:11]=[C:12]([CH3:15])[CH:13]=[CH:14][C:7]2=[N:6][C:5]=1[CH3:16].[C:17]1([CH3:29])[CH:22]=[CH:21][CH:20]=[C:19]([N:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)[CH:18]=1>C1(C)C=CC=CC=1>[C:17]1([CH3:29])[CH:22]=[CH:21][CH:20]=[C:19]([N:23]2[CH2:24][CH2:25][N:26]([CH2:2][CH2:3][C:4]3[C:9](=[O:10])[N:8]4[CH:11]=[C:12]([CH3:15])[CH:13]=[CH:14][C:7]4=[N:6][C:5]=3[CH3:16])[CH2:27][CH2:28]2)[CH:18]=1

Komponenten

4

Edukt 2

HCID 831111-(m-Tolyl)piperazineHCID 124149363-(2-Chloroethyl)-2,7-dimethyl-4H-pyrido[1,2-a]pyrimidin-4-one

Produkt 1

HCID 12414812HCID 12414812, VerbindungAusbeute 57,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A mixture of 2.2 g of 3-(2-chloroethyl)-2,7-dimethyl-4H-pyrido[1,2-a]pyrimidin-4-one, 5 g of 1-(m-tolyl)piperazine and 25 ml of toluene was refluxed for 30 hours. After completion of the reaction, the reaction mixture was filtered while hot and the filtrate was concentrated under reduced pressure. The residue was purified by means of column chromatography using alumina and recrystallized from a mixture of ethanol and isopropyl ether to give 2 g of the desired compound as pale yellow prisms, m.p. 115 - 116°C.

Aufarbeitung

  1. temperaturewas refluxed for 30 hours
  2. customAfter completion of the reaction
  3. filtrationthe reaction mixture was filtered while hot and the filtrate
  4. concentrationwas concentrated under reduced pressure
  5. customThe residue was purified by means of column chromatography
  6. customrecrystallized from a mixture of ethanol and isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-3659aeb59ddc440aba773ac9789dd5dc
Quelldatensatz
uspto-grants-1976_06
Patentnummer
US03960863

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