Reaktion #1687622

ord-60edf243ccb0493086a32b0c8e78a6a2

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeuntil acidic reaction
  2. 2
    FiltrationThe precipitate was filtered off
  3. 3
    Sonstigedried
  4. 4
    workup.DISSOLUTIONdissolved in methanol (25 ml)
  5. 5
    workup.ADDITION5% palladium on charcoal (0.6 g) was added
  6. 6
    FiltrationThe catalyst was filtered off
  7. 7
    Sonstigethe filtrate was evaporated to dryness
  8. 8
    SonstigeCrystallization from ethanol

Vorschrift

To a solution of 12 (1.93 g, 0.012 mol) in acetone (50 ml) was added hydrogen chloride in ether until acidic reaction. The precipitate was filtered off, dried, and dissolved in methanol (25 ml). 5% palladium on charcoal (0.6 g) was added, and the mixture was shaked overnight under 3 atm. of hydrogen pressure. The catalyst was filtered off and the filtrate was evaporated to dryness. Crystallization from ethanol yielded 0.63 g (0.0031 mol, 26%) of title product M.P. 168°-172° C. Anal. (C7H14ClN5) C, H, N.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: USRE036374uspto-grants-1999_11