N-(4-甲氧基-3-甲酰基苄基)亚氨基二乙酸的合成及表征

以2-甲氧基苯甲醛为原料，与浓盐酸和40％甲醛溶液进行氯甲基化反应，再用新制的无水碳酸钾作质子吸收剂、干燥的乙腈作溶剂，和亚氨基二乙酸二乙酯发生N-烷基化反应．然后用饱和Ba(OH)2水溶液进行水解得到N-(4-甲氧基-3-甲酰基苄基)亚氨基二乙酸的钡盐沉淀，最后用稀硫酸处理得到产物．通过改变各种实验因素，找到了合成标题化合物的最佳实验条件．该方法工艺简单、产率较高．所得化合物的结构通过^1H NMR和元素分析等进行了表征．     

Self-assembly of N-3-γ-pyridyl Aza[60]fulleroid on Au(111)

Self-assembled monolayers of novel C60 derivative, N-3-γ-pyridyl Aza[60]fulleroid (C60Py), on Au(111) were studied by a scanning tunneling microscope under ultrahigh vacuum (UHV). C60Py molecules were assembled on Au (111) via pyridyl nitrogen-Au interaction. The sole assembly of C60PY molecules on Au (III) only exhibited randoml aggregation of C60PY even the films were annealed at 50 and 105℃ .By co-assembling with benzyl mercaptan (BM), the C60PyBM films showed highly dense aggregation, but C60Py assemblies still had disordered structure. After the co-assembled C60Py-BM films were annealed at 50℃, BM molecules were partially desorbed, but the assembly of C60Py remained without obvious change. After the co-assembled C60Py-BM films were further annealed at 105℃, the C6oPy monolayers with ordered structure were obtained, while the BM molecules were nearly thoroughly desorbed from the surface. Here, the BM molecules play a key role as a surfactant in the formation of the ordered C6oPy monolayer.     

N-(4-羟苯基)维甲酰胺的生物素标记衍生物的合成

为了研究抗肿瘤药物N-(4-羟苯基)维甲酰胺(4-HPR)的作用机理和其生物学作用靶点,合成了4-HPR的生物素衍生物.采用全反式维甲酸与草酰氯反应生成酰氯,再与三乙胺成盐,然后将得到的酰基铵盐,与对氨基苯酚发生酰胺化反应,制得4-HPR.4-HPR与3-溴-1-丙醇烷基化反应得到含羟基链化合物,4-氨基丁酸与生物素发生酰胺化反应得到羧酸化合物.最后通过酯化反应将4-HPR与生物素连接得到目标化合物.该方法具有操作简单、反应条件温和以及产率较高等特点.     

对称的1.1─双(杂芳基)烷类的合成

从Ｎ─（ａ─苯并三唑烷基）氨基甲酸酯２与过量的２─甲基噻吩或２─甲基呋喃反应，得到各种１．１─双（杂芳基）烷类。产率很高。     

The identification of spiroacetals in the volatile secretions of two species of fruit fly (Dacus dorsalis,Dacus curcurbitae)

Summary Aeration extracts from femaleDacus cucurbitae and femaleDacus dorsalis have been shown to contain a variety of 2,8-dialkyl-1, 7-diaxospiro [5.5] undecanes together with N-3-methylbutylacetamide.     

N-[1,2,4]噻二唑[3,2-b]苯并噻唑苯甲酰亚胺的合成与晶体结构

报道了N-[1,2,4]噻二唑[3,2-b]苯并噻唑苯甲酰亚胺(3,C15H9N3OS2,Mr=311.37)的合成及晶体结构.晶体属于单斜晶系,空间群P21/c,晶胞常数:a=1.011 5(2)nm,b=1.184 8(2)nm,c=1.210 7(3)nm,α=90°,β=114.616°,γ=90°,Z=4,V=1.319 0(5)nm3,Dc=1.568 g/cm3,μ(MoK)=0.404mm-1,F(000)=640,241 9个可观察衍射点(I>2(σI)),R1=0.058 9,R2=0.120 1.X-衍射分析表明标题化合物为N-[1,2,4]噻二唑[3,2-b]苯并噻唑苯甲酰亚胺.     

N-（4-羟基苯基）-乙酰胺的合成及表征

以4-甲氧基苯胺为原料,经乙酰化、去甲基化两步反应合成得到了目标产物 N-（4-羟基苯基）-乙酰胺,并采用 IR、1H NMR 和13C NMR 对产物结构进行了表征。探讨了乙酰化反应时催化剂 AlCl3用量、反应温度及反应时间对 N-（4-甲氧基苯基）-乙酰胺产率的影响,以及去甲基化反应中催化剂 TBAB 用量、溴化氢用量、反应温度及反应时间对产物 N-（4-羟基苯基）-乙酰胺产率的影响。在最佳合成条件下,N-（4-羟基苯基）-乙酰胺的产率可达94.1%。