BAY-069是目前体外活性最强的支链氨基酸转氨酶1(BCAT1)抑制剂,但其报道的合成路线存在原料成本较高、总收率极低和中间体结构表征不充分等缺点。本研究基于已有合成路线,重点对其合成工艺中的Ullmann偶联反应进行了系统优化。以1-硝基...BAY-069是目前体外活性最强的支链氨基酸转氨酶1(BCAT1)抑制剂,但其报道的合成路线存在原料成本较高、总收率极低和中间体结构表征不充分等缺点。本研究基于已有合成路线,重点对其合成工艺中的Ullmann偶联反应进行了系统优化。以1-硝基萘(1)为起始原料,经过7步反应和手性色谱柱手性拆分合成目标化合物BAY-069。所有中间体和目标化合物均经1 H NMR,13 C NMR和HR-MS表征。以Ullmann偶联反应为主要优化步骤的路线,其优化后的总收率为11.0%(3b→(±)-BAY-069),是原总收率1.6%(3a→(±)-BAY-069)的6.9倍。展开更多
Heterocyclic selenium compounds were synthesized and their selfassembled monolayers (SAMs)on gold surface were reported.The heterocyclic selenium compounds are 4,5benzopiazselenole (BP) and anthra selenadiazol6...Heterocyclic selenium compounds were synthesized and their selfassembled monolayers (SAMs)on gold surface were reported.The heterocyclic selenium compounds are 4,5benzopiazselenole (BP) and anthra selenadiazol6,11dione (AS).The cyclic voltammetry results showed that the peaks of the oxidation and reduction of Fe(CN)3/46 almost disappeared after the Au electrode was covered by a monolayer of BP due to forming of SAMs,but AS did not.The reduction peak potentials of the BP and AS were 663mV and 659mV,respectively,in the Na2B4O7 solution with the modified gold electrode,while the reduction peaks potential of the BP and AS were 633mV and 704mV,respectively,with bare gold scanning in Na2B4O7ethanol solution,and the course was cortrolled by adsorption.展开更多
文摘BAY-069是目前体外活性最强的支链氨基酸转氨酶1(BCAT1)抑制剂,但其报道的合成路线存在原料成本较高、总收率极低和中间体结构表征不充分等缺点。本研究基于已有合成路线,重点对其合成工艺中的Ullmann偶联反应进行了系统优化。以1-硝基萘(1)为起始原料,经过7步反应和手性色谱柱手性拆分合成目标化合物BAY-069。所有中间体和目标化合物均经1 H NMR,13 C NMR和HR-MS表征。以Ullmann偶联反应为主要优化步骤的路线,其优化后的总收率为11.0%(3b→(±)-BAY-069),是原总收率1.6%(3a→(±)-BAY-069)的6.9倍。
文摘Heterocyclic selenium compounds were synthesized and their selfassembled monolayers (SAMs)on gold surface were reported.The heterocyclic selenium compounds are 4,5benzopiazselenole (BP) and anthra selenadiazol6,11dione (AS).The cyclic voltammetry results showed that the peaks of the oxidation and reduction of Fe(CN)3/46 almost disappeared after the Au electrode was covered by a monolayer of BP due to forming of SAMs,but AS did not.The reduction peak potentials of the BP and AS were 663mV and 659mV,respectively,in the Na2B4O7 solution with the modified gold electrode,while the reduction peaks potential of the BP and AS were 633mV and 704mV,respectively,with bare gold scanning in Na2B4O7ethanol solution,and the course was cortrolled by adsorption.
