Reaktion #412994
ord-abb4dffc39f2476d947189a08667135b
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
190°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling
- 2Filtrationinsoluble substance was remeved by filtration
- 3EinengenThe filtrate was concentrated to dryness under reduced pressure
- 4Sonstigethe residue was chromatographed on silica gel column
- 5WaschenA fraction eluted with the upper phase of a mixture of butanol:acetic acid:water (4:1:5 volume by volume)
- 6Einengenwas concentrated by dryness
Vorschrift
A mixture of diethyl 2-(5-phthalimidopentyl)-2-propylmalonate (6 g) and 26% hydrochloric acid (36 ml) was heated in a sealed tube at 190° C. for 4 hours. After cooling, insoluble substance was remeved by filtration. The filtrate was concentrated to dryness under reduced pressure and the residue was chromatographed on silica gel column. A fraction eluted with the upper phase of a mixture of butanol:acetic acid:water (4:1:5 volume by volume) was concentrated by dryness to give colorless sticky oil of the desired compound (yield 1.3 g).