Reaktion #318015

ord-c1252f81086244a2aaf7124be1d79e28

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe mixture was filtered through Celite
  2. 2
    Filtrationfilter aid
  3. 3
    Sonstigethe filtrate was evaporated
  4. 4
    Sonstigeto give a yellow/green oil
  5. 5
    Filtrationan insoluble precipitate filtered off
  6. 6
    Sonstigethe filtrate was evaporated in vacuo
  7. 7
    Sonstigeto give a yellow solid
  8. 8
    FiltrationTrituration with ether and filtration

Vorschrift

Intermediate 2 (13.1 g) was dissolved in acetic acid (150 ml) and hydrogenated over palladium on activated carbon (1.6 g) with stirring overnight. The mixture was filtered through Celite filter aid, and the filtrate was evaporated to give a yellow/green oil. The oil was taken up in methanol and an insoluble precipitate filtered off; the filtrate was evaporated in vacuo to give a yellow solid. Trituration with ether and filtration gave the title compound as a pale yellow solid (8.1 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07566786B2uspto-grants-2009_07