Reaktion #72545

ord-13879700969543ba963a03aca502957e

Lösungsmittel

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture is filtered
  2. 2
    Sonstigethe filtrate is then evaporated to dryness
  3. 3
    workup.STIRRINGThe residue is stirred in water overnight
  4. 4
    Filtrationfiltered
  5. 5
    Sonstigethe precipitate obtained
  6. 6
    Waschenis washed with water
  7. 7
    Sonstigeevaporated to dryness
  8. 8
    Filtrationfiltered
  9. 9
    Waschenwashed with ether
  10. 10
    Sonstigedried in vacuo at 40° C. under P2O5

Vorschrift

To a solution of the compound obtained in Step A (0.1448 mol) in glacial acetic acid (700 ml) there is added powdered zinc (0.8690 mol). The two-phase mixture is stirred at 40° C. for 8 hours. The reaction mixture is filtered and the filtrate is then evaporated to dryness. The residue is stirred in water overnight and filtered and the precipitate obtained is washed with water. The product is taken up in toluene and then evaporated to dryness, and is then taken up in ether, filtered, washed with ether and then dried in vacuo at 40° C. under P2O5 to yield the title product, which is used directly in the next Step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541412B2uspto-grants-2013_09