高纯度异恶草酮的合成工艺研究

Synthesis of Highly Pure Clomazone

介绍了改进的异恶草酮的合成工艺,以氯代特戊酰氯为原料,经肟化,合环,缩合反应得到异恶草酮粗品,之后经干燥HCl气体提纯得到高纯度的异恶草酮。通过研究反应条件对产品纯度的影响,使异恶草酮的纯度达到92%以上,经通入HCl气体提纯后,产品最终的纯度达到95%以上。总收率77.1%。产品结构经1 H NMR及GC-MS验证。

An improved synthetic process of clomazone was introduced.The crude product of clomazone was synthesized from 3-chloro-2,2-dimethyl propionyl chloride by oximation reaction,cyclization reaction and condensation reaction.Highly pure of clomazone was obtained by purifying the crude product with dry HCl gas.The influence of reaction conditions on the purity of the product was studied and the optimal purity reached above 92%.After purifying with HCl gas the purity of product reached above 95%.The overall yield was 77.1%.The product was confirmed by GC-MS and ^1H NMR.