Reaktion #93868

Reaktionsgleichung

potassium carbonate

O,O-diethyl chlorophosphate

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

→

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

Ausbeute 93.3%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationwas then filtered
2. 2
   SonstigeThe filtrate was evaporated to dryness
3. 3
   WaschenThe ether phase was washed with an aqueous solution of 100 g/l of sodium chloride
4. 4
   workup.ADDITIONwith an aqueous 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride
5. 5
   SonstigeThe solution was dried
6. 6
   workup.ADDITIONtreated with activated carbon
7. 7
   Filtrationfiltered
8. 8
   Sonstigeevaporated to dryness under reduced pressure

Vorschrift

7.7 g of potassium carbonate and 8.6 g of O,O-diethyl chlorophosphate were added to a solution of 11 g of 2-cyano-3-hydroxy-5-n-butoxy-thiophene in 150 ml of acetonitrile and the mixture was stirred for 16 hours at room temperature and was then filtered. The filtrate was evaporated to dryness and the residue was taken up in ethyl ether. The ether phase was washed with an aqueous solution of 100 g/l of sodium chloride and then with an aqueous 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride. The solution was dried, treated with activated carbon, filtered and evaporated to dryness under reduced pressure to obtain 15.5 g of 2-cyano-3-(diethoxyphosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.500.

Quelle