丙酮一步法合成甲基异丁基酮催化剂研究

用浸渍法制备了丙酮一步法合成甲基异丁基酮负载型催化剂，考察了载体的预处理温度、添加镧助剂对催化剂性能的影响；用BET法测定了催化剂的表面积；采用H2-O2滴定法测定Pd的分散度．结果发现，用经过1．023K焙烧过的Al2O3为载体的催化剂具有较好的催化性能，添加镧助剂后催化剂的分散度、活性有较大的提高．     

Selective reduction of aldehydes by a formic acid- trialkylamine- RuCl2(PPh3)3 system

In the presence of trialkylamine and formic acid RuCl₂(PPh₃)₃ selectively reduces aldehydes to the corresponding alcohols at room temperature. Other reducible groups are unaffected.     

内吸性杀菌剂三唑醇(酮)立体异构体的研究Ⅱ

三唑醇(Triadimenol,又称Baytan)是一种优良的内吸性广谱杀菌剂。谷类作物的种子经处理后,防治病虫害的效果极为突出,可增产粮食20%。此化合物化学名称为1-(对-氯苯氧基)-1-(1′,2′,4′-三氮唑-1′基)-3,3二甲基丁醇-2,结构式(Ⅰ)见后。由于分子中含有两个手性碳原子,故应有四种光学异构体。我们实验室曾分离出毫克量的三唑醇两个非对映异构体(A体和B体),生物测定表明两者的药效有明显差別,并确定有效者为A体。根据~1H-NMR中偶合常数,     

Phase Selectively Soluble Dendritic Derivative of 4-(Dimethylamino)- pyridine: An Easily Recyclable Catalyst for Baylis-Hillman Reactions

Among the reactions in which C-C bonds are formed, the Baylis-Hillman coupling of aldehydes with α, β-unsaturated carbonylic compounds is currently attracting much interest due to the atom economy, the mild conditions and the generation of functional groups1,2. Furthermore, compared to the Heck, Suzuki and other palladium catalyzed C-C bond forming reaction3, the Baylis-Hillman reaction can be promoted by using organic bases in the complete absence of any metal4. However, almost all the …     

The synthesis and crystal structure of metal complexes S-alkyl-N-(ferrocenyl-1-methyl-methylidene)-dithiocarbazate and the study on their quenching the luminescence ofruthenium(bipyridine)_~3(2+)

The cobalt, nickel, copper, zinc and cadmium complexes of S-methyl-N-(ferrocenyl-l-methyl-methylidene)-dithiocarbazate (H-LSM) and S-benzyl-N-(ferrocenyl-l-methyl-methylidene)-dithiocarbazate (H-LSB) were synthesized and the crystal structure of Cd[Fe-C(CH3) = NNCSS. (CH3)]2 was solved by X-ray diffraction. The crystal is in the orthorhombic system with space group Pbca, cell parameters a=19.741(3), b=19.924(5), c=15.452(4) A, and the final factors of R=0.032. The study on quenching the luminescence of Ru(bpy)3 by those complexes showed that bimolecular quenching constants obtained from the Stern-Vohner constant and the excited-state lifetime were related to the redox potential of the quencher. Linear relationship is shown in the plot of logkq vs. E1/2(Q+/Q). The main factor which influences the quenching rate constant and the redox potential is the coordinating ability of the metal in the complex.     

A New Saponin Transformed from Ginsenoside Rh1 by Bacillus subtilis

A novel saponin was isolated from the transformed products of ginsenoside Rh1 by Bacillus subtilis. It‘s structure was determined to be 3-O-β-D-glucopyranosyl-6-O-β-D-glucopyranosyl-20 (S)-protopanaxatriol on the basis of the spectral data.     

新型显色剂3,3,5,5''''-四甲基联苯胺分光光度法测定余氯的研究

本文报道了采用新型氧化还原剂3,3’,5,5’-四甲基联苯胺(TMB)测定水中总余氯的分光光度法,并对其灵敏度、稳定性、准确性作了较为详细的研究,探讨了分析条件,提出了分析方法。在pH≤2时,最大吸收峰为450 nm,表观摩尔吸光系数为6.89×10~4L·mol~(-1)·cm~(-1),可测范围为0.01～2.5 mg/L。与目前使用的传统显色剂邻联甲苯胺(DMB)相比较,具有灵敏度高,显色稳定,重现性好及使用安全等优点。     

Synthesis, characterization, antitumor activity of nickel(Ⅱ) and cobalt (Ⅱ) complexes of 2,2''''-diamino-4,4''''-bithiazole and their interaction with dGMP

New complexes,of bis(2,2'-diamino-4,4'-bithiazole)sulfate nickel(Ⅱ) and bis(2,2'-diami-no-4,4'-bithiazole)sulfate cobalt(Ⅱ),have been prepared.The complexes were characterized by infrared and UV-Vis spectroscopy,1H NMR,elemental analyses and molar conductivity.The effect of these complexes on the DNA synthesis of sarcoma 180 cells has been studied by the technique of isotopic liquid scintillation.The results indicated that complexes show ability to inhibit DNA synthesis of the tumor cells.In order to provide a molecular basis for understanding the biological effects,the probe,[trana-en2Os(η2-H2)](CF3SO3)2 (en,ethylenediamine) as a monitor was first used to explore interaction of the complexes with 2'-deoxyguanosine-5'-monophosphate (dGMP).     

石墨炉原子吸收分光光度法测定血清中铜

铜系人体内含有的微量元素。测定血清中Cu/Zn比值,有助于病因分析和提供诊断依据。目前,测定血清铜所用的仪器分析方法甚多。本法无需对血清样进行预处理,取样量仅20—50μl。碱金属和碱土金属卤化物无干扰。特征质量m。为5.6pg/0.0044A.S,回收率98～102%,变异系数1.7-2.7%。     

葡聚糖为载体的双亲型LDL吸附剂吸附动力学研究

合成了以葡聚为载体，同时具有亲水性磺酸基和疏水性胆固醇两类配基的新型低密度脂蛋白（LDL）吸附剂。通过对LDL纯溶液中吸附等温线的测试，比较了以Dextran G-75为载体的双亲型LDL吸附剂与单一亲水型磺酸基配基，单一疏水型胆固醇基吸附剂吸附量和亲和吸附系数的关系。对双亲型LDL吸附剂的吸附动力学进行了初步研究，在LDL溶液中，亲水型磺酸基，疏水型胆固醇配基，双亲型LDL吸附剂对LDL的吸附曲线基本上符合Langmuir吸附方程，另外通过高离子强度NaCl洗脱实验，测定了双亲型LDL吸附剂上具有的磺酸基与胆固醇两类基在对低密脂蛋白吸附过程中所起的配合效果，为下一步作用力机制研究提供了参考依据。