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目的:研究藁本内酯二聚体(化合物Ⅰ)的全合成工艺。方法:以邻苯二甲酸酐(化合物Ⅱ)为原料,经硼氢化钠还原得到苯酞(化合物Ⅲ)后经4步反应得到藁本内酯二聚体,经质谱、核磁共振氢谱(1H-NMR)和核磁共振碳谱(13C-NMR)进行表征。以催化剂、反应温度、反应时间为因素,收率为指标,采用正交试验优化第5步合成工艺,并进行验证。结果:第5步的最优合成工艺为在2%三氯化铝的催化下以温度150℃反应5 h。成功合成目标产物,验证试验平均收率为56.16%(RSD=1.23%,n=3);总的反应产率为24.4%,得到目标产物的纯度为99.4%。结论:成功合成藁本内酯二聚体,且本合成工艺稳定、质量可控。
Objective: To study the total synthesis of ligustilide dimer (compound Ⅰ). METHODS: Phthalic phthalic anhydride (compound Ⅱ) was used as raw material. After reduction with sodium borohydride to give phthalide (compound Ⅲ), the ligustilide dimer was obtained after 4 steps. The product was characterized by MS, 1H NMR NMR) and nuclear magnetic resonance (13C-NMR). Taking the catalyst, reaction temperature and reaction time as factors, yield as an index, the 5th step synthesis process was optimized by orthogonal test and verified. Results: The optimal synthesis process in the fifth step was the reaction at a temperature of 150 ℃ for 5 h under the catalysis of 2% aluminum trichloride. The target product was successfully synthesized. The average yield of the test was 56.16% (RSD = 1.23%, n = 3). The total reaction yield was 24.4%. The purity of the target product was 99.4%. Conclusion: The ligustilide dimers were successfully synthesized, and the synthesis process was stable and the quality was controlled.