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机构地区:[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
出 处:《河北师范大学学报(自然科学版)》2007年第4期495-496,502,共3页Journal of Hebei Normal University:Natural Science
基 金:国家自然科学基金(20472008)
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.The improved synthesis method of 2- methyl- 5,7- dihydrothieno [ 3,4- d ] pyrimidine 6,6 - dioxide starting from 4 - chloro- 2- methyl- 5,7 - dihydrothieno [ 3,4 - d ] pyrimidine 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 912 %, 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 (4-chloropyrimidine dioxide) : n (Zn) : n (NaOH) = 1 : 10:20, the reaction keeping at 100℃ for 2 h was the best reaction conditions.
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