Reaktion #2064

ord-2169f1be862948a3a9409a68450a60e7

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Sonstigethe EtOH was evaporated
  3. 3
    ExtraktionThe product was extracted into dichloromethane (5×50 ml)
  4. 4
    TrocknenThe organic layer was dried (Na2SO4)
  5. 5
    Einengenconcentrated

Vorschrift

A solution of NaOH (4.00 g, 100 mmol) in water (50 ml) was added to a solution of ethyl 3,3-bis(diethoxyphosphinyl)propionate (32.6 g, 87 mmol) in EtOH (100 ml), and heated at 80° C. for 1 hour. After cooling, the EtOH was evaporated, and the residue was acidified to methyl orange with 12N HCl. The product was extracted into dichloromethane (5×50 ml). The organic layer was dried (Na2SO4) and concentrated to give the title compound (28.8 g, 96%) as a viscous oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05728650uspto-grants-1998_03