在线阅读 --自然科学版 2007年4期《2-甲基-5,7-二氢噻吩并[3,4-d]嘧啶6,6-二氧化物的合成新方法》
2-甲基-5,7-二氢噻吩并[3,4-d]嘧啶6,6-二氧化物的合成新方法--[在线阅读]
张宝华1, 史兰香2
1. 石家庄学院物理系, 河北石家庄 050035;
2. 石家庄学院化工学院, 河北石家庄 050035
起止页码: 495--496,502页
DOI:
摘要
对4-氯-2-甲基-5,7-二氢噻吩并[3,4-d]嘧啶6,6-二氧化物为原料合成2-甲基-5,7-二氢噻吩并[3,4-d]嘧啶6,6-二氧化物的方法进行了改进.与文献报道的Pd-C/H2脱氯方法相比,用新的甲苯-锌粉-氢氧化钠溶液-TBAB体系常压脱氯,简便易行,避免了加氢脱氯的危险性,降低了成本,产物收率达92%.对反应条件进行了优化:甲苯为溶剂,TABA为相转移催化剂,n(4-氯嘧啶二氧化物)∶n(Zn)∶n(NaOH)=1∶10∶20,温度100 ℃,反应时间2 h.

A New Preparation Method of 2-methyl-5,7-dihydrothieno [3,4-d]Pyrimidine 6,6-dioxide
ZHANG Bao-hua11, SHI Lan-xiang22
1. Department of Physics, Shijiazhuang University, Hebei Shijiazhuang 050035, China;
2. College of Chemical Engineering, Shijiazhuang University, Hebei Shijiazhuang 050035, China
Abstract:
The improved synthesis method of 2-methyl-5,7-dihydrothieno[3,4-d]pyrimidine 6,6-dioxide starting from 4-chloro-2methyl-5,7-dihydrothienopyrimidine 6,6-dioxide was reported.In this technology,the chlorine atom displacement reaction carried out in toluene-zinc-sodium hydroxide-TBAB system and the yield was up to 92 %,the operations were simple and easy,the danger from hydrogen reaction was avoided,the cost of product was decreased.The experimental results showed the toluene as a solvent,the TBAB as a phase transfer catalyst,n(4chloropyrimidine dioxide)∶n(Zn)∶n(NaOH)=1∶10∶20,the reaction keeping at 100 ℃ for 2 h was the best reaction conditions.

收稿日期: 2006-10-21
基金项目: 国家自然科学基金(20472008)

参考文献: