Reaktion #93866

Reaktionsgleichung

potassium carbonate

O,O-diethyl chlorothiophosphate

2-cyano-3-hydroxy-5-n-butoxy-thiophene

→

2-cyano-3-(diethoxythiophosphoryloxy)-5-n-butoxy-thiophene

Ausbeute 80.6%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

7 g of potassium carbonate and 9.4 g of O,O-diethyl 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 filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with benzene yielded 14 g of 2-cyano-3-(diethoxythiophosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.525.

Quelle