Reaktion #72574

ord-487f88ec2cbf40ff8accf80c7ce6dbb9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture is heated
  2. 2
    Temperaturat reflux for two hours
  3. 3
    SonstigeThe solid formed
  4. 4
    Filtrationis then filtered off
  5. 5
    Waschenwashed with water
  6. 6
    Trocknendried in vacuo in the presence of P2O5 and at 40° C. overnight

Vorschrift

Sodium sulphate (78.3 g) is added to a solution of trichloroacetaldehyde hydrate (32.5 mmoles) in water (100 ml). To the resulting suspension there are added a solution of 3-[2-(4-amino-phenyl)ethyl]oxazolidin-2-one in water (20 ml) and concentrated HCl solution (2.83 ml). A solution of hydroxylamine hydrochloride (95 mmoles) in water (50 ml) is then added. The reaction mixture is heated at reflux for two hours. The mixture is then cooled to ambient temperature. The solid formed is then filtered off, washed with water and dried in vacuo in the presence of P2O5 and at 40° C. overnight 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