Reaktion #93869

Reaktionsgleichung

potassium carbonate

O,O-dimethyl chlorophosphate

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

→

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

Ausbeute 76.8%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationwas filtered
2. 2
   SonstigeThe filtrate was evaporated to dryness under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue was dissolved in ether
4. 4
   WaschenThe ether solution was washed with water containing 100 g/l of sodium chloride
5. 5
   workup.ADDITIONwith 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride
6. 6
   TrocknenThe ether phase was dried
7. 7
   workup.ADDITIONtreated with activated carbon
8. 8
   Filtrationfiltered
9. 9
   Einengenconcentrated to dryness

Vorschrift

7.7 g of potassium carbonate and 7.7 g of O,O-dimethyl 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 20° C. and was filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was dissolved in ether. The ether solution was washed with water containing 100 g/l of sodium chloride and then with 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride. The ether phase was dried and treated with activated carbon, filtered and concentrated to dryness to obtain 12.5 g of 2-cyano-3-(dimethoxyphosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.511.

Quelle