Reaktion #929456

ord-807451b7222f4154af48a2ea8602344b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture was refluxed
  2. 2
    Temperaturunder heating for an hour
  3. 3
    Extraktionextracted with ethyl acetate
  4. 4
    WaschenThe organic layer was washed with an aqueous sodium hydrogencarbonate solution
  5. 5
    Trocknena saturated brine and dried over sodium sulfate
  6. 6
    workup.DISTILLATIONThe solvent was distilled away under reduced pressure

Vorschrift

To a solution of ethyl 4-(2-benzyloxyphenyl)-2-methoxycarbonylamino-2-methylbutanoate (5.2 g) in tetrahydrofuran (135 ml), under a nitrogen atmosphere, lithium borohydride (0.59 g) was added and the mixture was refluxed under heating for an hour. Then, a 2N hydrochloric acid (6.6 ml) was added thereto and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with an aqueous sodium hydrogencarbonate solution and a saturated brine and dried over sodium sulfate. The solvent was distilled away under reduced pressure to give the subject compound (4.6 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06372800B1uspto-grants-2002_04