Reaktion #2039990

ord-2f313e17b67044f0876bf7fa1656f5e5

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwas washed with 1N sodium hydroxide aqueous solution and saturated brine successively
  2. 2
    Trocknendried over sodium sulfate anhydride
  3. 3
    Filtrationfiltrated
  4. 4
    SonstigeThe solvent was evaporated out
  5. 5
    Sonstigethe residue was purified by silica gel column chromatography (silica gel 85 g, chloroform:methanol=100:1)

Vorschrift

N,N-Diisopropylethylenediamine (0.79 g) was added to the intermediate (a) (2.62g) obtained in Example 28. After being stirred for 2 hours at 70° C., the reaction mixture, with chloroform added thereto, was washed with 1N sodium hydroxide aqueous solution and saturated brine successively, dried over sodium sulfate anhydride, and then filtrated. The solvent was evaporated out and the residue was purified by silica gel column chromatography (silica gel 85 g, chloroform:methanol=100:1), thereby yielding 1.45 g of the aimed compound as white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06114325uspto-grants-2000_09