Reaktion #4467

ord-683c16909174462faf1b49adbea715f3

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was heated
  2. 2
    Temperaturat reflux for 17 hours
  3. 3
    Sonstigethe volatiles removed on a flash evaporator
  4. 4
    ExtraktionThe product was extracted with ether
  5. 5
    Extraktionthe ether extract
  6. 6
    Waschenwashed with brine
  7. 7
    Trocknendried over magnesium sulfate
  8. 8
    Einengenconcentrated in vacuo

Vorschrift

To 100 ml of a 50:50 (v/v) methanol/water solution containing 14.35 g of potassium carbonate, was added n-butyl 2-tert-butoxyacetate (6.50 g, 0.0346 mol). The mixture was heated at reflux for 17 hours and the volatiles removed on a flash evaporator. The remaining solution was cooled to approximately 0° C. and acidified to pH 3-4 with cold 50% aqueous hydrogen chloride. The product was extracted with ether, the ether extract washed with brine and dried over magnesium sulfate, then concentrated in vacuo to give the title compound as a yellow liquid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04725620uspto-grants-1988_02