抗帕金森病药雷沙吉兰的合成工艺优化

以1-茚酮(1)为原料,在室温下与盐酸羟胺作用制得2,3-二氢-1H-茚-1-酮肟(2)。然后以乙醇作溶剂,经镍铝合金还原制得1-氨基茚满(3),并应用星点设计-响应面法对还原工艺进行了优化。随后再与对甲苯磺酸炔丙酯反应制得N-炔丙基-1-氨基茚满(4)。最后经L-酒石酸拆分、甲磺酸成盐得到雷沙吉兰(5)。以1为原料计算总收率约为31%。     

异香兰素化学合成的研究进展

异香兰素,化学名3-羟基-4-甲氧基苯甲醛,是一种非常重要的香料和食品药品领域应用广泛的医药中间体。近年来市场对异香兰素需求量不断增大,使得异香兰素的合成与应用研究也成为热点。简述异香兰素当前主要的应用状况,综述异香兰素不同的化学合成路线及进展,对各路线进行分析评价,展望利用生物技术、植物细胞培养技术等方法生产异香兰素的研究发展方向。     

Alcaligenes sp. CGMCC2428产威兰胶的分批发酵动力学模型

利用分批发酵研究Alcaligenes sp. CGMCC2428产微生物多糖威兰胶的合成特性,结果表明威兰胶的合成和菌体生长模型为部分偶联型.菌体和威兰胶质量浓度分别达到3.30和26.50 g/L,威兰胶对细胞干质量得率系数（YP/X）为8.20.根据分批发酵实验结果采用Logistic方程、Luedeking-Piret方程和Luedeking-Piret相似方程,得到了描述Alcaligenes sp. CGMCC2428生长、威兰胶以及葡萄糖底物消耗分批发酵动力学模型.同时改变初始葡萄糖质量浓度,实验数据与模型预测值进行了比较拟合,平均相对误差小于10%,表现出很好的适用性.     

三环酮的合成研究发展

本文简述了开瑞坦、去羧氯雷他定药物,并且综述其典型中间体三环酮的合成工艺路线.     

质子泵抑制剂兰索拉唑的合成

以2,3-二甲基-4-硝基吡啶-N-氧化物为原料,通过2个“一锅法”,经4步反应合成兰索拉唑.改进的合成路线缩短了合成工艺流程提高了产品收率,反应条件相对温和.总收率达到39.2％,高于文献报道的18.8％,适合工业化生产.     

3-乙氧基-4-甲氧基苯甲醛的合成

以乙醇为溶剂,以异香兰素和溴乙烷为原料,以碘化钾为催化剂,碳酸钾为缚酸剂,合成3-乙氧基-4-甲氧基苯腈中间体3-乙氧基-4-甲氧基苯甲醛。考察了原料摩尔比、反应体系的压力、反应温度及时间等因素对产品收率的影响。最佳合成工艺条件为:异香兰素45. 6g(0. 30mol),异香兰素与溴乙烷摩尔比为1. 00:1. 15,0. 5MPa下于85℃下反应5h,3-乙氧基-4-甲氧基苯甲醛的收率达到97%以上。     

用锆英砂合成锆石颜料的研究

本研究采用碱熔融法分解锆英砂,分解产物经氢卤酸处理后直接用于颜料的合成,合成的钒锆兰、镨锆黄和铁锆红颜料可以作为高温色釉的色料。     

雷替曲塞合成工艺综述

雷替曲塞被广泛用于治疗晚期结肠、直肠癌。按不同的起始原料对抗癌药物雷替曲塞的合成方法进行了总结。     

咪唑并[1，2-b]哒嗪

介绍了咪唑并[1,2-b]哒嗪的合成方法、用途、生产及需求.以3,6-二录哒嗪为原料,经氨化、环合、脱氯得咪唑并[1,2-b]哒嗪。咪唑并[1,2-b]哒嗪是合成头孢类抗生素的侧链中间体,因合成难度较大,成为国内开发头孢唑兰的瓶颈.     

印度兰的合成与应用

本文介绍了一种新型的酞菁钴染料印度兰的合成机理、工艺流程、检测方法及其产品的应用,并介绍了国内印度兰的发展现状和市场需求。     

Coumarin-Rasagiline Hybrids as Potent and Selective hMAO-B Inhibitors,Antioxidants, and Neuroprotective Agents

The frequency, complexity and morbidity of neurodegenerative diseases make them a great challenge for nowadays medicine. Most of the treatments currently used for Parkinson's disease – the second most prevalent – are only symptomatic. Therefore, it is urgent to develop drugs that are able to act simultaneously on different targets, being able to stop neuronal death and promote the recovery of neuronal populations already affected. In this work, we studied the activity of a series of hybrid molecules, which combine the structure of both coumarin and an alkynylamine group inspired on rasagiline, as MAO inhibitors, antioxidants and neuroprotective agents. Half of the studied hybrids turned out to be selective monoamine oxidase B (hMAO-B) inhibitors in the low micro/nanomolar range, demonstrating that positions 3 (compounds 1–3 ) and 7 (compounds 8 and 10 ) of the coumarin scaffold are the most suitable for the incorporation of the alkynylamine chain. All the studied compounds proved to be capable of neutralizing free radicals (DPPH). Finally, the 4-(but-2-yn-1-ylamino)coumarin ( 5 ) showed neuroprotective effects on glial cells and the 4-methyl-7-(pent-2-yn-1-ylamino)coumarin ( 8 ) inhibited intraneuronal ROS production as well.     

Study of oil soluble polymers as drag reducers

This investigation was undertaken to find the most effective material which would reduce the friction coefficient in turbulent flow when added in small quantities to oil pipelines. For this purpose, a series of oil-soluble polymers, namely homopolymers and copolymers of alkyl methacrylates, alkyl acrylates, and alkyl styrenes were synthesized. Emulsion polymerization techniques were used. Commercially available alkyl methacrylate and alkyl acrylate monomers were used in the synthesis. Monomeric alkyl styrenes were synthesized and structures established prior to polymerization. Intrinsic viscosities were measured and viscosity average molecular weights were calculated for several of the homopolymers synthesized in this study. Reduction of factional drag and resistance to shear degradation were measured by pumping a solution of the polymer in a hydrocarbon solvent through a pipe and recording the pressure drop across the pipe. Drag-reducing properties of several of the polymers were correlated in terms of their viscosity average molecular weights. Drag reduction of poly (isodecyl methacrylate) was studied in various hydrocarbon solvents. Drag-reducing behavior of polymers prepared in this study exhibited a strong dependence on molecular weight; increasing the molecular weight increased the drag reduction for a given polymer concentration and pipe size. Several of these polymers were found to be superior to commercially available polyisobutylene as drag reducers, especially in terms of shear stability.     

几种土壤处理除草剂室内生物活性及对甘薯的安全性测定

[方法]采用室内盆栽法和土壤处理法测定8种药剂的活性及对甘薯的安全性。[结果]供试的8种药剂对反枝苋及稗草均具有较高除草活性;异丙甲草胺、二甲戊灵、氟乐灵、乙草胺、仲丁灵、异草松6种药剂的选择性系数分别为6.15、5.78、3.04、2.57、2.29、2.19,安全性好;草酮和扑草净选择性系数为0.70、1.24,安全性差。[结论]异丙甲草胺、二甲戊灵、氟乐灵、乙草胺、仲丁灵及异草松可以开展田间试验,进一步确定在甘薯田应用的可行性,扑草净和草酮不宜在甘薯田应用。     

Effect of enzyme inactivation on the extracted soybean meal and oil

The objective was prevention of lipoxygenase activity prior to oil extraction in order to obtain a meal of superior flavor quality and a crude oil of superior oxidative stability. Accordingly, experiments were performed in which soybeans were heated at various moisture contents and times to inactivate the enzyme system. Once the optimal conditions were determined, heat treated and raw beans were extracted in a laboratory system designed to simulate conditions in commercial solvent extraction and the component oil and meal were evaluated. Oxidative stability of the oil from heat-treated beans was increased as determined by the Swift stability test and an organoleptic evaluation. Similarly, organoleptic blandness ratings of the heat-treated meal were also superior to the meal produced from raw beans. It was concluded that steam heat treatment of soybeans prior to extraction was beneficial to quality of both oil and flake.     

POLYCYCLIC AROMATIC HYDROCARBONS BIOACCUMULATION AND BIOTRANSFORMATION PRODUCTS IN TROUT EXPOSED THROUGH FOOD PELLETS

Polycyclic aromatic hydrocarbons (PAHs) were previously measured in whole small finfish (< 30 cm) or in the internal organs relative to the rest of tissues, as well as in muscle, liver, and gonads of larger finfish, collected offshore in the Northwest Atlantic. Alkylated naphthalenes (NA) were more abundant than phenanthrenes (PA), while fluoranthene (FL), pyrene (PY), and chrysene (CH) were also detected in some cases. Bioaccumulation pointed to uptake by respiration and, probably by a dietary contribution, especially for benthic species. Therefore, speckled trout were exposed to PA, FL, and PY through food and the parent PAH and their respective metabolites were analyzed. Trout maintained at 10°C were fed daily for 10 weeks with pellets spiked with 0.33–0.38 μg of each PAH per g fish. Muscle, internal organs, and bile of fish were analyzed by HPLC every 2 weeks, for up to 14 weeks. The concentration of PA was always higher than that of FL. No phase I or phase II metabolites were detected for either compound, even in the bile. Concentrations and total tissue burdens were higher in the internal organs than in the muscle for PA and FL. The highest levels of PA equivalent to 5 days' feeding were present in internal organs on week 10. Levels of PY were lower than levels of FL in internal organs and muscle. The amounts of PY-glucuronide in whole gall bladder bile were higher than amounts of PY in any whole compartment. PY-glucuronide was also detected in internal organs. Comparison will be made to a short-term exposure of winter flounder to 5 μg/g of the same three PAHs.     

安克锰锌在荔枝树上施用的残留代谢消解规律与安全性评价

安克锰锌是烯酰吗啉两个异构体和代森锰锌组成的多元混合制剂。试样经粉碎、溶剂浸泡提取、混合柱净化,用气相色谱测定烯酰吗啉和代森锰锌母体(CS2),液相色谱测定代谢物乙撑硫脲(ETU)。仪器最低检出量:烯酰吗啉为1.436×10-12g,代森锰锌母体1.326×10-10g,ETU2.5×10-10g,最低检出浓度依次为0.02、0.025、0.02mg/kg,方法回收率依次为86.4%～90.8%、89.2%～95.9%、89.10%～95.13%;标准偏差为0.53～4.34;变异系数为0.58%～4.62%。安克锰锌在果皮中的消解方程广西和广东分别为C=1.2719e-0.1975T和C=1.045e-0.1972T,半衰期(T/2)均为3.5d;土壤中分别为C=0.8734e-0.1187T和C=0.6171e-0.1146T,半衰期(T/2)=6d;最高剂量250倍、最多施3次,最短距收期7d,在果肉中均未检出,果皮和土壤中的残留仅分别为0.1385～0.1745mg/kg和0.3105～0.3415mg/kg,均低于欧共体规定代森锰锌MRL值0.5mg/kg。     

桂西铝工业尾矿库安全性研究

广西西部地区是全国重要的铝工业基地之一,境内建有多个尾矿库并且还有新的尾矿库正在建设中。文章对桂西铝地区工业尾矿库安全性能情况进行评述,指出引起安全事故发生的最主要因素:(1)尾矿库溃坝、坝塌;(2)尾矿库库坝漏水、渗水;列出相关的解决措施,并提出几点建议。     

Solubilities and diffusion coefficients of carbon dioxide in poly(vinyl acetate) and polystyrene

Solubilities of carbon dioxide in poly(vinyl acetate) (PVAc) were measured at temperatures from 313.15 to 373.15 K and pressures up to 17.5 MPa. Diffusion coefficients of carbon dioxide in PVAc were also measured at 313.15 K and pressures up to 7 MPa. Solubilities and diffusion coefficients of carbon dioxide in molten polystyrene (PS) were studied at temperatures from 373.15 to 473.15 K and pressures up to 20 MPa. An apparatus using a magnetic suspension balance (MSB) was constructed for the measurements. The solubilities in the PVAc and the PS were in good agreement with literature data. The solubility in both polymers were correlated with the Sanchez and Lacombe equation of state to within an average relative deviation of 3.6 and 1.6% for PVAc and PS systems, respectively. The diffusion coefficients in PS were correlated with free volume theory of Kulkarni and Stern to within 10% of relative average deviation.     

Countermeasures against alkali-related problems during combustion of biomass in a circulating fluidized bed boiler

The purpose of this work was to study different ways to mitigate alkali-related problems during combustion of biomass in circulating fluidized beds. Wood chips and wood pellets were fired together with straw pellets, while the tendency to agglomerate and form deposits was monitored. In addition to a reference case, a number of countermeasures were applied in related tests. Those were addition of elemental sulphur, ammonium sulphate and kaolin to a bed of silica sand, as well as use of olivine sand and blast-furnace slag as alternative bed materials. The agglomeration temperature, composition and structure of bed-ash samples were examined. The flue-gas composition, including gaseous alkali chlorides, was measured in the hot flue gases and in the stack. Particles in the flue gas were collected and analysed for size distribution and composition. Deposits were collected on a probe in hot flue gases and their amount and composition were analysed. Addition of kaolin was found to be the best method to counteract the agglomeration problem. The deposition problem is effectively counteracted with addition of ammonium sulphate, while kaolin is too expensive to be used commercially against deposits, and sulphur is less effective than ammonium sulphate.     

The examination of fats and fatty acids for toxic substances

The chick edema disease factor was found to be present in a number of distillates and residues that were obtained during the production of commercial fatty acids. The raw materials from which the toxic samples were produced included inedible animal tallows, acidulated vegetable oil foots, and oils recovered from tin plate manufacture. The chick edema factor was found to be present in several oleic acids and in a triolein. Twenty stearic acid samples which were examined were nontoxic. The nonurea adduct-forming fatty acids that were isolated from commercial oleic acids and various distillates and residues from the manufacture of commercial fatty acids were found to be toxic to weanling rats even after hydrogenation. Analysis of the nonurea-adducting monomers that were isolated from a fatty acid by-product distillate indicated the presence of cyclic structures.