摘要
目的优化取代四氢萘类化合物的合成工艺,重点考察10%Pd/C对关键中间体合成的影响。方法平行试验比较10%Pd/C和三乙基硅烷催化羰基还原反应,并对实验结果进行总体分析;对10%Pd/C催化还原采用正交设计法,考察反应物与10%Pd/C的投料比例及溶剂对收率的影响。结果 10%Pd/C催化羰基还原的成本明显低于三乙基硅烷,且收率高,杂质少,易处理;正交试验证实,催化剂与反应物的投料比例对反应的影响最为显著。结论实验证实,利用10%Pd/C催化还原关键中间体,使得取代四氢萘类化合物的合成路线更加符合工业生产的要求。
Objective To optimize the synthesis of substituted tetrahydronaphthalene and investigate the influence of 10% Pd/C catalyst in the synthesis of key intermediate. Methods A parallel test was carried out to compare the catalytic activity of triethyl silicane and the 10% Pd/C catalyst, including the total analysis of experimental result . And orthogonal experimental design was used and the influence of solvent and reactant ratio on the yield were investigated. Results The cost of the 10% Pd/C eatalyst was obvious- ly lower than that of triethyl silieane,with high yield, little impurity easy effluent disposal. Orthogonal test confirms that the ratio of re- actant and catalystthe was the most significant factor. Conclusion The experiments proved that the optimal preparation procedure was much more available for industrial production using the 10% Pd/C as a catalyst.
出处
《药学实践杂志》
CAS
2012年第1期35-37,共3页
Journal of Pharmaceutical Practice
基金
国家自然科学基金(20972187)
关键词
取代四氢萘
合成
正交设计
substituted tetrahydronaphthalene
synthesis
orthogonal design