反应详情

温度

20 °C

11.2 g of potassium carbonate and 12.8 g of O,O-dimethyl chlorothiophosphate were added to a solution of 11.2 g of 2-cyano-3-hydroxy-5-methyl-thiophene in 200 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 a 7-3 cyclohexane-ethyl acetate mixture yielded 18.7 g of 2-cyano-3-(dimethoxythiophosphoryloxy)-5-methyl-thiophene with a refractive index of nD20 =1.539.

1. filtrationwas then filtered
2. customThe filtrate was evaporated to dryness
3. customthe residue was chromatographed over silica gel
4. washElution with a 7-3 cyclohexane-ethyl acetate mixture