N-bromobutanimide → HCID 67148260, Verbindung

HRID 2426266Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2426266
[C:1]([O:9][C:10]1[C:20](=[O:21])[N:14]2[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:13]2=[N:12][C:11]=1[C:22]([O:24][CH3:25])=[O:23])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Br:26]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[C:1]([O:9][C:10]1[C:20](=[O:21])[N:14]2[CH2:15][CH2:16][CH2:17][CH2:18][CH:19]([Br:26])[C:13]2=[N:12][C:11]=1[C:22]([O:24][CH3:25])=[O:23])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 67184N-bromobutanimideHCID 67147764HCID 67147764, Verbindung

Produkt 1

HCID 67148260HCID 67148260, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5943Carbon TetrachlorideLösungsmittel

Versuchsvorschrift

A mixture of methyl 3-(benzoyloxy)-4-oxo-4,6,7,8,9,10-hexahydropyrimido[1,2-a]azepine-2-carboxylate, N-bromo-succinimide (2 eq.) and α,α′-azoisobutyronitrile (0.45 eq.) in carbon tetrachloride was stirred under reflux for 14 hour. The mixture was cooled to room temperature, the succinimide was filtered off and the solvent was removed under reduced pressure. Methyl 3-(benzoyloxy)-10-bromo-4-oxo-4,6,7,8,9,10-hexahydropyrimido[1,2-a]azepine-2-carboxylate was obtained after flash chromatography (eluents petroleum ether/ethyl acetate, 8:2) as a pale yellow solid.

Aufarbeitung

  1. temperatureunder reflux for 14 hour
  2. filtrationthe succinimide was filtered off
  3. customthe solvent was removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-3a6e79591a784a7fb1906d8698bb590f
Quelldatensatz
uspto-grants-2011_06
Patentnummer
US07968553B2

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