由双甲酮合成王朝酮

Synthesis of Dynascone From Dimedone

以双甲酮为原料,先经过还原得到双甲烯酮,然后与膦叶立德发生Wittig反应以增长侧链,进行环氧化后并开环重排得到目标产物王朝酮,反应的总产率为19.0%。目标产物用IR,1HNMR表征。探讨了反应温度对中间体产率的影响,研究表明:对于反应过程1,当温度为65℃时,中间体1产率达到56.7%;对于反应过程3,当温度为-10℃时,中间体3产率达到79.0%。

At first, 5,5-dimethyl-2-cyclohexen-l-one was prepared via reduction reaction with dimedone as starting material, and then targeted product dynascone was synthesized via Wittig reaction to extend side chain, via epoxidation and rearrangement. The overall yield was 19%. The product was characterized by IR,1HNMR. Effect of reaction temperature on the yield of intermediate product was investigated. The results show that,the yield can reach to 56.7% at 65℃ for process 1; the yield can reach to 79.0% at-10℃ for process 3.