Reaktion #350216

ord-8bbd155d40c14abfb93aac1291fe82c1

Lösungsmittel

Reaktionsbedingungen

Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationwas then filtered
  2. 2
    SonstigeThe filtrate was evaporated to dryness
  3. 3
    Sonstigethe residue was chromatographed over silica gel
  4. 4
    WaschenElution with benzene

Vorschrift

7 g of potassium carbonate and 8 g of O,O-dimethyl chlorothiophosphate were added to a solution of 9.8 g of 2-cyano-3-hydroxy-5-n-butoxy-thiophene in 150 ml of acetonitrile and the mixture was stirred for 24 hours at 20° C. and was then filtered. The filtrate was evaporated to dryness and the residue was chromatographed over silica gel. Elution with benzene yielded 11 g of 2-cyano-3-(dimethoxythiophosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 =1.5375.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04155996uspto-grants-1979_05