以硫脲和氯乙酸为原料,在无溶剂和350 W微波辐射4 m in条件下,缩合生成中间体2,4-噻唑烷二酮(Ⅰ)产率91.5%;随后在无溶剂和400 W微波辐射5 m in条件下,通过V ilsm e ier甲酰化反应,生成中间体4-氯-5-甲酰基噻唑-2(3H)-酮(Ⅱ),产率86.7%...以硫脲和氯乙酸为原料,在无溶剂和350 W微波辐射4 m in条件下,缩合生成中间体2,4-噻唑烷二酮(Ⅰ)产率91.5%;随后在无溶剂和400 W微波辐射5 m in条件下,通过V ilsm e ier甲酰化反应,生成中间体4-氯-5-甲酰基噻唑-2(3H)-酮(Ⅱ),产率86.7%;最后以正丙醇为溶剂,450 W微波辐射7 m in条件下,成环得到5-氨基-噻唑[4,5-d]嘧啶-2(3H)-酮(Ⅲ),产率80.5%。反应总产率为63.9%。合成产物与中间体的结构经1HNMR,MS和元素分析确认。展开更多
A series of 2 amimo 3 cyano 7,7 dimethyl 4 aryl 5 oxo 5,6,7,8 tetra 4H chromenes were synthesized in the absence of catalyst. Their structures were determined by IR, 1H NMR, and single crystal X ray diffraction.
By taking 3 chloro 4 methyl aniline as raw material,two solvent mixtures of naphtha and petroleum ether in a certain proportion,and through sulfonation 2 amino 4 chloro 5 toluene sulfonic acid was synthesized.The yiel...By taking 3 chloro 4 methyl aniline as raw material,two solvent mixtures of naphtha and petroleum ether in a certain proportion,and through sulfonation 2 amino 4 chloro 5 toluene sulfonic acid was synthesized.The yield of product was about 90%,and the recovery of solvents was over 95%.展开更多
文摘以硫脲和氯乙酸为原料,在无溶剂和350 W微波辐射4 m in条件下,缩合生成中间体2,4-噻唑烷二酮(Ⅰ)产率91.5%;随后在无溶剂和400 W微波辐射5 m in条件下,通过V ilsm e ier甲酰化反应,生成中间体4-氯-5-甲酰基噻唑-2(3H)-酮(Ⅱ),产率86.7%;最后以正丙醇为溶剂,450 W微波辐射7 m in条件下,成环得到5-氨基-噻唑[4,5-d]嘧啶-2(3H)-酮(Ⅲ),产率80.5%。反应总产率为63.9%。合成产物与中间体的结构经1HNMR,MS和元素分析确认。
文摘A series of 2 amimo 3 cyano 7,7 dimethyl 4 aryl 5 oxo 5,6,7,8 tetra 4H chromenes were synthesized in the absence of catalyst. Their structures were determined by IR, 1H NMR, and single crystal X ray diffraction.
文摘By taking 3 chloro 4 methyl aniline as raw material,two solvent mixtures of naphtha and petroleum ether in a certain proportion,and through sulfonation 2 amino 4 chloro 5 toluene sulfonic acid was synthesized.The yield of product was about 90%,and the recovery of solvents was over 95%.
