反应详情

温度

20 °C

7 g of potassium carbonate and 9.5 g of O,O-diethyl chlorothiophosphate were added to a solution of 7 g of 2-cyano-3-hydroxy-5-methyl-thiophene in 100 ml of acetone and the mixture was stirred for 15 hours at 20° C. and was then filtered. The filtrate was evaporated to dryness and the residue was chromatographed over silica gel. Elution with an 8-2 cyclohexane-ethyl acetate mixture yielded 11.2 g of 2-cyano-3-(diethoxythiophosphoryloxy)-5-methyl-thiophene with a refractive index of nD20 =1.534.

1. filtrationwas then filtered
2. customThe filtrate was evaporated to dryness
3. customthe residue was chromatographed over silica gel
4. washElution with an 8-2 cyclohexane-ethyl acetate mixture