Synthesis and characterization of new polyamides derived from 1,3-bis[4-(4-aminophenoxy)phenyl]adamantane

Several new polyamides were synthesized by direct polycondensation of the 1,3-bis[4-(4-aminophenoxy)phenyl]adamantane ( I ) with various dicarboxylic acids. The polyamides had inherent viscosities and number-average molecular weights (M_n) of 0.46–0.96 dL/g and 28,000–109,000, respectively. All polyamides III had good solubilities and were soluble in N-methyl-2-pyrrolidone (NMP), N,N-dimethylacetamide (DMAc), N,N-dimethylformamide (DMF), and pyridine. Polyamides had tensile strengths of up to 72.3 MPa, elongation to breakage values of up to 10.2%, and initial modulus of up to 2.1 GPa. Their glass transition temperatures were found to be 228–269°C and 252–307°C using differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA), respectively. The melting temperature of III_f was observed at 318°C using DSC. The temperatures of polyamides III at a 5% weight loss ranged from 395 to 435°C in air and from 400 to 450°C in a N₂ atmosphere. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 68:315–321, 1998     

改性分子筛催化异构化合成金刚烷的研究

以桥式四氢双环戊二烯(endo-TCD)为反应物,表面负载固体超强酸ZrO2-SO42-的REY,USY,S i-MCM-41等分子筛为异构化反应催化剂,采用间歇反应方式合成了金刚烷。分子筛表面负载ZrO2-SO42-有助于提高金刚烷收率。采用SZ/REY催化剂考察了反应温度、氢压、ZrO2负载量等因素对endo-TCD异构化反应及产物分布的影响。在催化剂为SZ(20%)/REY,催化剂/反应物(m/m)=0.625,反应温度250℃,氢压1.5 MPa的条件下反应3 h,得到了收率为22.77%的金刚烷,挂式四氢双环戊二烯(exo-TCD)和金刚烷总选择性高达95%。     

固载化AlCl_3催化合成金刚烷

以固载化AlCl3为催化剂催化桥式四氢双环戊二烯(endo-TCD)异构化合成金刚烷。采用N2吸附、原子吸收和化学分析方法对载体的比表面积、孔分布和催化剂中氯化物负载量进行了表征;考察了载体类型、催化剂颗粒大小、反应温度、单釜反应时间对催化剂性能的影响。实验结果表明,以γ-Al2O3为载体制备的固载化AlCl3催化剂具有较高的活性和较好的金刚烷选择性;升高反应温度、延长单釜反应时间及使用大颗粒催化剂有利于提高金刚烷选择性。在以20～40目γ-Al2O3为载体的固载化AlCl3催化剂7.5mL、endo-TCD0.5g、环己烷用量20mL、反应温度413K、H2压力2.5MPa、单釜反应时间4h的条件下,endo-TCD转化率为100.0%,金刚烷选择性达24.6%,反应12次后金刚烷选择性降至14.0%。该催化剂可重复使用,失活原因是生成的焦油覆盖了催化剂表面的强酸中心。     

含4-噻唑啉酮环的新金刚烷类化合物的合成及抗癌活性研究

以1-金刚烷甲酸为原料,通过酯化、肼解制得1-金刚烷甲酰肼,1-金刚烷甲酰肼再与芳香醛反应得到相应的酰腙,最后以苯和DMF为溶剂,酰腙与巯基乙酸脱水环化成2-芳基-3-(1-金刚烷甲酰胺基)-4-噻唑啉酮类化合物,并利用IR、1HNMR、13CNMR、ESI-MS和元素分析对7个目标化合物的结构进行了表征。用MTT方法评价了它们在体外对HepG-2,A549-1和231-2 3种癌细胞株的体外生长抑制活性。结果表明,所合成的7个新化合物均具有潜在的体外抑制癌细胞生长活性。     

Antimicrobial and Hypoglycemic Activities of Novel N-Mannich Bases Derived from 5-(1-Adamantyl)-4-substituted-1,2,4-triazoline-3-thiones

The reaction of 5-(1-adamantyl)-4-ethyl or allyl-1,2,4-triazoline-3-thione with formaldehyde solution and various 1-substituted piperazines yielded the corresponding N-Mannich bases. The newly synthesized N-Mannich bases were tested for in vitro inhibitory activities against a panel of Gram-positive and Gram-negative bacteria and the yeast-like pathogenic fungus Candida albicans. Six compounds showed potent antibacterial activity against one or more of the tested microorganisms, while two compounds exhibited moderate activity against the tested Gram-positive bacteria. None of the newly synthesized compounds were proved to possess marked activity against Candida albicans. The oral hypoglycemic activity of six compounds was determined in streptozotocin (STZ)-induced diabetic rats. Four compounds produced significant strong dose-dependent reduction of serum glucose levels, compared to gliclazide at 10 mg/kg dose level (potency ratio > 75%).