Reaktion #412994

ord-abb4dffc39f2476d947189a08667135b

Reaktionsbedingungen

Temperatur
190°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Filtrationinsoluble substance was remeved by filtration
  3. 3
    EinengenThe filtrate was concentrated to dryness under reduced pressure
  4. 4
    Sonstigethe residue was chromatographed on silica gel column
  5. 5
    WaschenA fraction eluted with the upper phase of a mixture of butanol:acetic acid:water (4:1:5 volume by volume)
  6. 6
    Einengenwas 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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04443365uspto-grants-1984_04