Reaktion #722651

ord-f4eff23435464980b23bd8f911901e47

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: US06187821B1uspto-grants-2001_02