Reaktion #1612504

ord-687fd6b2c5b540e88747899bb1ee27e0

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThen evaporated the solvent
  2. 2
    workup.ADDITIONthe residue diluted with H2O (5 ml)
  3. 3
    Extraktionextracted with ethyl acetate
  4. 4
    Extraktionextracted with ethyl acetate
  5. 5
    Waschenthe organic phase washed with brine
  6. 6
    Sonstigedried
  7. 7
    Einengenconcentrated under vacuo

Vorschrift

tert-butyl 2-(6-(4-(diethoxyphosphoryl)phenyl)pyridin-3-yl)propan-2-ylcarbamate (5.3 g, 11.8 mmol) was dissolved in HCl in dioxane (30 ml), the mixture was stirred at 50° C. for 4 hours. Then evaporated the solvent and the residue diluted with H2O (5 ml), extracted with ethyl acetate and the water phase was adjusted to pH=9 with 1N aqueous NaOH, extracted with ethyl acetate and the organic phase washed with brine and dried, concentrated under vacuo to give the product 33-g.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09079930B2uspto-grants-2015_07