反応 #93863

反応方程式

potassium carbonate

O,O-diethyl chlorothiophosphate

2-cyano-3-hydroxy-5-ethylthio-thiophene

→

2-cyano-3-(diethoxythiophosphoryloxy)-5-ethylthio-thiophene

収率 86.8%

溶媒

acetonitrile

反応条件

後処理

1. 1
   ろ過was filtered
2. 2
   その他The filtrate was evaporated to dryness
3. 3
   その他the residue was chromatographed over silica gel
4. 4
   洗浄Elution with an 8-2 cyclohexane-ethyl acetate mixture

実験手順

7 g of potassium carbonate and 9.4 g of O,O-diethyl chlorothiophosphate were added to a solution of 9.3 g of 2-cyano-3-hydroxy-5-ethylthio-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 and the residue was chromatographed over silica gel. Elution with an 8-2 cyclohexane-ethyl acetate mixture yielded 14.6 g of 2-cyano-3-(diethoxythiophosphoryloxy)-5-ethylthio-thiophene with a refractive index of nD20 = 1.5635.

出典