Sec-Butylamine → HCID 19881217, Verbindung

HRID 745308Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 745308
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16]([Cl:20])=[N:17][C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2.[CH:21]([NH2:25])([CH2:23][CH3:24])[CH3:22]>CN(C)C=O>[ClH:20].[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16]([NH:25][CH:21]([CH2:23][CH3:24])[CH3:22])=[N:17][C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2

Komponenten

4

Edukt 2

HCID 24874Sec-ButylamineHCID 46787202-Chloro-6,7-dihydro-9,10-dimethoxy-4H-pyrimido[6,1-a]isoquinolin-4-one

Produkt 1

HCID 19881217HCID 19881217, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 9,10-dimethoxy-6,7-dihydro-2-chloro-4H-pyrimido(6,1-a)isoquinolin-4-one (2.5 g), sec-butylamine (10 ml) and dimethylformamide (2 ml) is heated under reflux for 5 hours. The solvent and excess amine are distilled under reduced pressure. The residue is treated with water. A white solid precipitates and is collected by filtration. The precipitate is crystallized from methylene chloride-ether mixture, yield 2.10 g. The crystals are dissolved in dichloromethane and treated with a solution of etheral hydrochloric acid. The hydrochloride is crystallized from ethanol-ether mixture, m.p. 218°-225° C.

Aufarbeitung

  1. temperatureunder reflux for 5 hours
  2. distillationThe solvent and excess amine are distilled under reduced pressure
  3. additionThe residue is treated with water
  4. customA white solid precipitates
  5. filtrationis collected by filtration
  6. customThe precipitate is crystallized from methylene chloride-ether mixture, yield 2.10 g
  7. dissolutionThe crystals are dissolved in dichloromethane
  8. additiontreated with a solution of etheral hydrochloric acid
  9. customThe hydrochloride is crystallized from ethanol-ether mixture, m.p. 218°-225° C.

Quellen und Nachweise

ORD-Eintrag
ord-e7d5709a5ff440d987630d6c477c43da
Quelldatensatz
uspto-grants-1986_07
Patentnummer
US04598148

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