Reaktion #86502
ord-a1a37df2a7c047c4a48b07db83119876
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeAfter removal of acetonitrile in vacuum
- 2workup.DISSOLUTIONthe resulting solid was dissolved in methylene chloride
- 3Waschenwashed with water, saturated Na2S2O3, saturated sodium bicarbonate, and brine
- 4Trocknenand then the organic layers dried over sodium sulfate
- 5Filtrationfiltered
- 6EinengenThe filtrate was concentrated under reduced pressure
Vorschrift
A mixture of 2-(1-bromopropyl)-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (3.46 g, 12.3 mmol) and N-iodosuccinimide (4.15 g, 18.4 mmol) in acetonitrile (100 mL) was stirred at 80° C., under nitrogen, overnight. After removal of acetonitrile in vacuum, the resulting solid was dissolved in methylene chloride, washed with water, saturated Na2S2O3, saturated sodium bicarbonate, and brine; and then the organic layers dried over sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure to provide the desired product (4.53 g, 90.4%). LCMS calculated for C12H13BrIN2O (M+H)+: m/z=406.9. Found: 407.1.