Reaktion #550576

ord-f4bc4a8622e144d6810bd8801cd3bea2

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturunder reflux for an hour
  3. 3
    Extraktionextracted with diethyl ether (10 ml×2)
  4. 4
    WaschenThe extract was washed with 5% aqueous sodium thiosulfate solution (5 ml×5)
  5. 5
    TrocknenThe solution was dried over magnesium sulfate
  6. 6
    Sonstigeevaporated under reduced pressure

Vorschrift

Pyridinium hydrobromide perbromide (1.82 g) was added to a solution of ethyl 2-methoxyimino-3,3-dimethoxybutyrate (syn isomer, 1.0 g) in dry tetrahydrofuran (10 ml) and heated under reflux for an hour. The resultant solution was poured into water (30 ml) and extracted with diethyl ether (10 ml×2). The extract was washed with 5% aqueous sodium thiosulfate solution (5 ml×5) and a saturated aqueous solution of sodium chloride (10 ml×1) successively. The solution was dried over magnesium sulfate and evaporated under reduced pressure to give ethyl-2-methoxyimino-3,3-dimethoxy-4-bromobutyrate (syn isomer, 2.02 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04518774uspto-grants-1985_05