摘要
以吲哚(1)、甲醛(2)和二甲胺(3)为原料,固载蒙脱土(MMT)/路易斯酸(L)为催化剂,通过微波辐射合成了芦竹碱(4),其结构经1H NMR确证。考察了MMT/L、反应温度、反应时间、溶剂和物料比r[n(1)∶n(2)∶n(3)]对4产率的影响。结果表明:在最优反应条件[甲醇为溶剂,MMT/Zn Cl2为催化剂,MMT/Zn Cl218 mg,1 1mmol,r=1.0∶1.3∶1.3,于50℃反应10 min]下合成4,产率93.8%。MMT/Zn Cl2循环使用3次,4产率60.0%
Gramine( 4) was synthesized by microwave-assist method from indole( 1),formaldehyde( 2) and dimethylamine( 3),using immobilized montmorillonite /Lewis acid as the catalyst. The structure was confirmed by1 H NMR. The effects of catalyst,reaction temperature,reaction time,solvent and molar ratio{ r[n( 1) ∶ n( 2) ∶ n( 3) ]} on the yield of 4 were investigated. The optimum conditions of synthesis 4 at 50 ℃ for 10 min were as follows: methanol as the solvent,MMT / Zn Cl2 as the catalyst,MMT / Zn Cl20. 15 mmol,1 1 mmol,r = 1. 0 ∶ 1. 3 ∶ 1. 3. The yield of 4 was 93. 8% under the optimum conditions. The yield of 4 was 60. 0% after MMT / Zn Cl2 used for three times.
出处
《合成化学》
CAS
CSCD
2015年第6期543-546,共4页
Chinese Journal of Synthetic Chemistry
基金
贵州师范大学研究生创新基金资助项目[硕创2014(11)]
贵州省科技创新人才团队建设项目{黔科合人才团队[2014]4006号}