降低萘呋胺酯草酸盐原料药中杂质方法的研究

目的:降低萘呋胺酯草酸盐原料药中的单个未知杂质和主要杂质C[3-(1-萘基)-2-(1-萘甲基)丙酸-2-二乙胺基乙酯草酸盐]的含量.方法:再次氢化、酯化物高真空蒸馏、成盐后重结晶、酸性条件下水解、氧气破坏性氧化.结果:主要杂质A和C含量达到英国药典标准,排除了原料药水解、氧化和氢化不完全引入单个未知杂质的可能.结论:高真空蒸馏然后重结晶是降低C杂质含量的可行方法.     

dl-丹参素的合成

目的探讨dl-丹参素新的合成工艺。方法以3，4-二羟基苯甲醛为起始原料，经过苄基保护、Darzens反应、Lewis酸选择性开环、NaBH4还原、水解、氢化6步反应得到丹参素。结果与结论目标化合物以一丹参素的结构经^1H-NMR确证，总收率为48．4％。     

2-巯基-5-甲氧基苯并咪唑合成工艺的研究

目的改进2-巯基-5-甲氧基苯并咪唑的合成工艺。方法以对氨基苯甲醚为起始原料,采用醋酸硝酰作硝化剂进行硝化;采用雷尼镍催化加氢法进行还原。结果制得了奥美拉唑中间体2-巯基-5-甲氧基苯并咪唑,总收率78.5%。结论值得推广到工业化生产。     

The fatty acyl chain composition of human normal and leukaemic lymphocytes and its modulation by specialised hydrogenation

Thirty species of fatty acyl chain have been quantitatively identified in human normal peripheral blood lymphocytes (four donors) and lymphocytes circulating in eight patients with chronic lymphocytic leukaemia (CLL). Towards the aim of influencing cell behaviour by lowering membrane fluidity, reaction conditions for catalytic hydrogenation at physiological temperature and pH have been established that effect reduction of the unsaturated species, and preferentially the polyunsaturated forms, but this has not yet been accomplished without killing the cells. That saturation of ethylenic linkages per se is the cause of death is indicated by separate findings showing that the lymphocytes are capable of withstanding hydrogen gas at the requisite high pressure (9 atm.) or exposure alone to the rhodium catalyst [chlorotris (sodium diphenylphosphinobenzene-m-sulphonate)-rhodium(I) tetrahydrate]. It remains feasible that future use of these two agents in combination under milder conditions to produce much lower degrees of hydrogenation than those reported here will permit the cells to survive.Concerning fatty acyl chain composition, the lymphocytes from most of the patients exhibited an inversion in the level of palmitic and stearic acid. A consistently abnormal pattern exhibited by the patients was a rise in oleic acid and a fall in arachidonic acid content. This same alteration has been demonstrated elsewhere in transformed/neoplastic cell types and hence it could well represent phenotypic expression in the CLL lymphocyte of malignant change.Fatty acyl chain composition remained unchanged in lymphocytes reconstituted after cryopreservation in liquid nitrogen.     

降血糖药物那格列奈的合成研究

目的 合成速效降血糖药物那格列奈H型结晶。方法 以4-异丙基苯甲酸为原料,用RaneyNi催化氢化制备反式4-异丙基环己甲酸,再经酰氯化得到酰氯。结果酰氯和D-苯丙氨酸缩合合成那格列奈B型晶,再用水为溶剂进行转晶型得到那格列奈H型晶,总收率53．6％。结论最终产物经熔点和IR测定证明为那格列奈H型结晶。     

Spherical Silica Modified with Magnesium and Ruthenium—Synthesis,Characterization and Catalytic Properties

The design of different bimetallic catalysts is an important area of catalytic research in the context of their possible applications in the cascade processes, meeting the requirements of the so-called green chemistry. In this study, such catalysts were obtained by the incorporation of magnesium species into spherical silica, which was in the next step covered with porous silica and modified with ruthenium species. The structure and chemical composition of the materials obtained were determined by XRD measurements, low temperature N₂ adsorption/desorption, SEM, ICP-OES and XPS methods. The catalytic activities of materials obtained were tested in 2-propanol decomposition and hydrogenation of levulinic acid. The results obtained confirmed the successful coverage of nanospheres with porous silica. A much higher concentration of ruthenium species was found on the surface of the catalysts than in their bulk. The opposite relationship was observed for magnesium species. The modification of nanospheres with silica had a positive effect on the catalytic activity of the materials obtained. For the most active sample, i.e., Ru/NS/3Mg/NS, 49% of levulinic acid conversion in its hydrogenation process was reported with γ-valerolactone as the only product.     

异麦芽酮糖的氢化反应过程

异麦芽（酮）糖醇（帕拉金糖醇）是由异麦芽酮糖通过加氢反应还原而成的.探讨了在密闭的反应釜内温度、压力、初始糖质量浓度及搅拌转速等工艺参数对加氢反应速度的影响,得到了气液两相在催化剂表面接触反应的较好控制条件,为压力11MPa,温度范围120～130℃,初始糖质量浓度20g/dL,搅拌转速500r/min.在上述条件下,反应2h后转化率可达99.5%,所得到的异麦芽酮糖醇达到FAO质量标准的要求.     

用正交试验法改进黄藤素氢化工艺

目的 :探索提高延胡索乙素收率的黄藤素氢化工艺条件。方法 :本文采用正交实验法选择黄藤素最佳氢化工艺 ,以硼氢化钾为还原剂 ,酒精为溶剂 ,加入适量从黄藤粗碱提取黄藤素后的母液的提取物 (以下简称 C提取物 ) ,水浴加热反应。结果 :C提取物对提高延胡索乙素收率的作用具有显著性 (P<0 .0 1) ,可使延胡索乙素收率提高 5 %左右。结论 :实验证明最佳的氢化工艺条件为 A2 B1 C3,即硼氢化钾与黄藤素用量之比为 1:5 ,酒精浓度为 70 % ,溶剂用量为黄藤素的 10倍。     

5-硝基-2-氯甲基呋喃的制备

以糠醛为原料,通过硝化、水解、硼氢化钠还原和氯代等反应合成出5-硝基-2-氯甲基呋喃。总产率为57.6%,运用GC-MS、NMR对产物进行了表征。     

六氢假紫罗酮的新合成法

氯异戊烯与亚异丙基丙酮在相转移催化条件下缩合得2和3,以氢氧化钠代替 DBU 在分馏塔内使副产物3异构化为2,并对缩合的条件进行了研究,2经格氏、重排及氢化等反应得六氢假紫罗酮(1),纯度98%,总收率43.4%。