以D-氨基葡萄糖盐酸盐、间硝基苯甲酸和对甲基苯甲酸为原料,先将氨基葡萄糖的羟基加以保护,然后以N,N-二环已基碳二亚胺(DCC)为脱水剂,合成N-硝基苯甲酰基-1,3,4,6-四-O-乙酰基-2-脱氧-β-D-氨基葡萄糖.产品结构经傅里叶变换红外光谱(FT...以D-氨基葡萄糖盐酸盐、间硝基苯甲酸和对甲基苯甲酸为原料,先将氨基葡萄糖的羟基加以保护,然后以N,N-二环已基碳二亚胺(DCC)为脱水剂,合成N-硝基苯甲酰基-1,3,4,6-四-O-乙酰基-2-脱氧-β-D-氨基葡萄糖.产品结构经傅里叶变换红外光谱(FT-IR)及核磁共振氢谱(1 H NMR)表征确认.研究表明:1,3,4,6-四-O-乙酰基-2-脱氧-β-D-氨基葡萄糖、DCC和间硝基苯甲酸/对甲基苯甲酸的摩尔比为1∶1.5∶1.5,反应温度为40℃,反应时间为4h为最佳反应条件.展开更多
以对氨基水杨酸为起始原料,经过甲基化、硫氰化、还原乙基化、氧化、水解得到4-氨基-5-乙磺酰基-2-甲氧基苯甲酸。探讨了甲基化反应和硫乙基引入方法问题,并对各步反应合成条件进行了优化。改进后工艺总收率达55%,目标化合物和各中间体...以对氨基水杨酸为起始原料,经过甲基化、硫氰化、还原乙基化、氧化、水解得到4-氨基-5-乙磺酰基-2-甲氧基苯甲酸。探讨了甲基化反应和硫乙基引入方法问题,并对各步反应合成条件进行了优化。改进后工艺总收率达55%,目标化合物和各中间体经IR,1 H NMR和MS等确证结构。展开更多
4′-acetylbenzo-15-crown-5thiosemicarbazone was synthesized with high yield (94%)via the reaction of 4′-acetylbenzo-15-crown-5 and thiosemicarbazide under the microwave irradiation and hydrochloric acid as the cataly...4′-acetylbenzo-15-crown-5thiosemicarbazone was synthesized with high yield (94%)via the reaction of 4′-acetylbenzo-15-crown-5 and thiosemicarbazide under the microwave irradiation and hydrochloric acid as the catalyst.Its structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic crystal system,P-1 space group,a=9.5470(19)?,b=13.637(3)?,c=16.029(3)?,α=75.33(3)°,β=83.62(3)°,γ=70.99(3)°,V=1097.8(7)s assembled into supramolecule structure by intermolecular hydrogen bonds.展开更多
文摘以D-氨基葡萄糖盐酸盐、间硝基苯甲酸和对甲基苯甲酸为原料,先将氨基葡萄糖的羟基加以保护,然后以N,N-二环已基碳二亚胺(DCC)为脱水剂,合成N-硝基苯甲酰基-1,3,4,6-四-O-乙酰基-2-脱氧-β-D-氨基葡萄糖.产品结构经傅里叶变换红外光谱(FT-IR)及核磁共振氢谱(1 H NMR)表征确认.研究表明:1,3,4,6-四-O-乙酰基-2-脱氧-β-D-氨基葡萄糖、DCC和间硝基苯甲酸/对甲基苯甲酸的摩尔比为1∶1.5∶1.5,反应温度为40℃,反应时间为4h为最佳反应条件.
文摘4′-acetylbenzo-15-crown-5thiosemicarbazone was synthesized with high yield (94%)via the reaction of 4′-acetylbenzo-15-crown-5 and thiosemicarbazide under the microwave irradiation and hydrochloric acid as the catalyst.Its structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic crystal system,P-1 space group,a=9.5470(19)?,b=13.637(3)?,c=16.029(3)?,α=75.33(3)°,β=83.62(3)°,γ=70.99(3)°,V=1097.8(7)s assembled into supramolecule structure by intermolecular hydrogen bonds.
