二甲氧基乙酰乙酸甲酯的合成研究

以二甲氧基乙酸甲酯和乙酸甲酯为主要原料，经甲醇钠催化，制备药物尼伐地平中间体二甲氧基乙酰乙酸甲酯。通过考察原料摩尔比、催化剂用量、加料温度、反应温度和反应时间等因素对收率的影响，得到了最佳反应条件。二甲氧基乙酰乙酸甲酯的收率可达53．3％。     

降压新药西尼地平杂质Ⅰ的制备

以西尼地平为起始原料,活化MnO2为氧化剂,一步法制备了2,6-二甲基-4-(3-硝基苯基)吡啶-3,5-二甲酸3-(2-甲氧基)乙酯5-(3-苯基)-2(E)-丙烯酯(记为西尼地平杂质Ⅰ).经实验优化,制备西尼地平杂质Ⅰ的最适宜条件为:m(西尼地平):m(MnO2)=1.00:1.24,甲苯为溶剂,105℃下反应1 h.反应得到西尼地平杂质Ⅰ收率为92.3％,经高效液相色谱面积归一化法检测后,纯度达到99.2％.产物结构经HRMS,1HNMR、13CNMR以及FTIR进行确认.该反应实现了西尼地平绿色高效直接转化西尼地平杂质Ⅰ.     

抗癌药乐伐替尼的合成工艺改进

乐伐替尼是一种口服的多受体酪氨酸激酶(RTK)抑制剂。以对硝基苯基氯甲酸酯为原料,经两次酰化反应得到关键中间体1-(2-氯-4-羟基苯基)-3-环丙基脲,再在叔丁醇钾和无水碳酸钠作用下与4-氯-7-甲氧基喹啉-6-甲酰胺缩合,得到目标化合物乐伐替尼。通过1 HNMR、FTIR对中间体和目标化合物的结构进行了表征,并对其合成工艺进行了改进,优化了酰化反应的原料投料比和反应温度、缩合反应的碱试剂投料比。通过改进,目标化合物乐伐替尼总产率为51.2%,降低了反应成本,提高了反应产率,符合绿色化学的要求。     

抗肿瘤药Lenvatinib相关杂质的合成

为了控制原料药乐伐替尼质量,分别以化合物1和3为原料,经酰化、胺化,成脲得到2和5,然后这两个中间体发生亲核取代反应得到乐伐替尼杂质A:4-(3-氯-4-(3-环丙基脲)苯氧基)-7-甲氧基喹啉-6-甲酸甲酯。杂质A经碱水解,得到杂质B:4-(3-氯-4-(3-环丙基脲)苯氧基)-7-甲氧基喹啉-6-羧酸。两个杂质均为工艺杂质,其结构经核磁、质谱和元素分析确证。同时,对两个杂质产生的原因及机理进行了分析,为今后乐伐替尼的工业化生产提供指导。     

巴伐朗尼大放异彩：切割、磨边与CNC设备推陈出新。尽显综合技术实力

巴伐朗尼（BAVELLONI）推出了一系列新产品，大大提高建筑玻璃与家具玻璃的加工效率与灵活性。巴伐朗尼先前已推出了用于太阳能玻璃加工的设备型号，其预处理解决方案也完全满足光伏玻璃的技术要求。产品类型的整合更提高了设备的自动化程度和程序控制。     

抗肿瘤药乐伐替尼相关杂质的合成

为了控制乐伐替尼的质量,本文以4-氨基-3-氯苯酚为起始原料,经酰化、成脲得到中间体1-(2-氯-4羟基苯基)-3-环丙基脲(4),然后该中间体与4-氯-7-甲氧基喹啉-6-甲酰胺(5)发生亲核取代反应得到乐伐替尼的有关杂质4,4'-[4,4'-羰基双(脲二基)双(3-氯-4,1-次苯基)]双(氧)双(7-甲氧基喹啉-6-羧酰胺),该杂质为工艺杂质,其结构经核磁、质谱和元素分析确证。同时,对该杂质产生的原因及机理进行了分析,为今后乐伐替尼的工业化生产提供指导。     

降纤酶治疗纤维蛋白原增高的短暂性脑缺血发作临床观察

目的探讨降纤酶治疗伴有纤维蛋白原增高的短暂性脑缺血发作患者的临床疗效及安全性。方法随机选择在我院神经内科住院经确诊的短暂性脑缺血发作56例,男性35例、女性21例,年龄51～87岁(平均65岁),分为降纤酶治疗组35例,尼膜地平对照组21例。结果降纤酶对短暂性脑缺血发作患者的疗效好,起效时间快,显著优于尼膜地平(P<0.01)。结论降纤酶治疗纤维蛋白原增高的短暂性脑缺血发作患者疗效确切,且无明显不良反应。     

固体分散技术在西尼地平片工艺中的应用

目的:通过应用固体分散增溶技术提高难溶性药物西尼地平片的溶出度[1]。方法:通过将难溶性药物西尼地平先制成固体分散体后,再制备西尼地平片,并采用高效液相色谱法测定其体外释放度。结果:通过固体分散体制备的西尼地平片可以显著提高西尼地平的溶出度[2]。结论:固体分散技术可以显著提高西尼地平片的溶出度,且质量稳定,重现性好。     

格拉司通集团将持续推动中国建筑节能事业

全球玻璃深加工业的资深企业，格拉司通集团与旗下泰姆、巴伐朗尼两大品牌，多年来一直在分享行业信息，促进全球玻璃行业整体发展方面发挥着重要的作用。     

尼泊金酯合成新方法

研究了1GHz、50mW·cm~2微波连续辐照常压回流条件下直接酯化制备尼泊金酯反应体系。与常规回流方式相比,微波方式使反应速度提高10倍以上、产率明显提高而温度未变,探讨了其作用机制与分子间氢键及分子缔合性有关。     

Formation of Apatite Coatings on an Artificial Ligament Using a Plasma- and Precursor-Assisted Biomimetic Process

A plasma- and precursor-assisted biomimetic process utilizing plasma and alternate dipping treatments was applied to a Leed-Keio artificial ligament to produce a thin coating of apatite in a supersaturated calcium phosphate solution. Following plasma surface modification, the specimen was alternately dipped in calcium and phosphate ion solutions three times (alternate dipping treatment) to create a precoating containing amorphous calcium phosphate (ACP) which is an apatite precursor. To grow an apatite layer on the ACP precoating, the ACP-precoated specimen was immersed for 24 h in a simulated body fluid with ion concentrations approximately equal to those in human blood plasma. The plasma surface modification was necessary to create an adequate apatite coating and to improve the coating adhesion depending on the plasma power density. The apatite coating prepared using the optimized conditions formed a thin-film that covered the entire surface of the artificial ligament. The resulting apatite-coated artificial ligament should exhibit improved osseointegration within the bone tunnel and possesses great potential for use in ligament reconstructions.     

电容吸附法海水脱钙研究

将改性的LSX分子筛按一定比例掺加到活性炭中,制成复合电极(CE),测定了其在不同的吸附时间、分子筛含量、电压、电极间距、电极片质量下,该复合电极对钙离子的去除率。同时比较了其与普通活性炭电极(AC)对钙离子的吸附能力。结果表明,在Ca2+/Na+溶液中,钙离子吸附量提高了1.08倍,在Ca2+/Mg2+溶液中,钙离子吸附量提高了0.6倍,在Ca2+/K+溶液中,吸附量提高了7.45倍,在海水溶液中,吸附量提高了2倍。     

Calcium sulfate hemihydrate scaling threshold enhancement by magnesium ion augmentation

Efficient high temperature distillation of sea water cannot be realized without development of scale control systems for calcium sulfate. This paper describes a new concept of scaling threshold enhancement based on complexing a portion of dissolved sulfate ion in the form of stable MgSO^o ion pairs. Complexing may be accomplished by augmentation of feed water with magnesium ion recovered and recycled from distilling plant blowdown. This “tying up” of sulfate ion results in higher solubility levels of calcium sulfate. Magnesium ion augmentation at levels up to three times ambient results in markedly improved resistance to hemihydrate scaling in natural sea water. Significantly higher levels of operating temperature and concentration factor may be achieved by this technology.     

Nucleation of Hydroxyapatite Crystal through Chemical Interaction with Collagen

The nucleation of hydroxyapatite (HAp) crystal through chemical interaction with collagen was investigated. A collagen membrane was soaked in a supersaturated simulated body fluid (1.5 SBF) solution with ion concentrations at 1.5 times that of normal simulated body fluid (1.0 SBF). A few carbonate-containing HAp crystals were formed mostly on the edge-side of the collagen membrane after 4 weeks. In the Fourier-transform infrared spectometry (FTIR) results, the carboxylate band of the collagen membrane showed red chemical shifts after the formation of HAp crystals, which coincided well with the decrease of the calculated bond orders of the carboxylate group when chelated with a calcium ion, which emulated the first-step nucleation of HAp crystal on the carboxylate group of collagen. The result implies that the binding of a calcium ion to the carboxylate group of collagen is one of the key factors for the nucleation of HAp crystals in a 1.5 SBF solution.     

离子交换法回收土霉素及废水处理的研究

采用离子交换法回收制药废水中的土霉素,通过考察离子交换液的pH、离子交换树脂转型的选择、流量、解吸剂的浓度等因素的影响,确定了提取土霉素的适宜条件.试验结果表明,该法提取制药废水中的土霉素是可行的.同时,对离子交换余液进行微电解-生化处理,制药废水最终达到了国家排放标准.     

Effect of calcium ion and montmorillonite clay on bitumen displacement by water on a glass surface

Experiments were conducted to study the effect of calcium ion and montmorillonite clay on bitumen displacement by an aqueous phase on a glass surface. Upon exposure to an aqueous environment containing calcium ion and clays, a thin coating of bitumen on a glass surface displaced spontaneously in the inward radial direction. The initially circular bitumen disk took the shape of a spherical droplet. The dynamic and static contact angles of bitumen on the glass surface were estimated by measuring the contact radius of bitumen with time. The dynamic and static contact angles in the presence of calcium ion and clays are compared with the case when no calcium ion and clays are present. At pH 9, the static contact angle decreased significantly in the presence of calcium ion having a concentration higher than 25 ppm. For a given temperature and at a pH of 9, the initial dynamic angle variation with time was affected less by the presence of clays than with the case of calcium addition. There was no synergetic effect on the dynamic and static angles due to the presence of both calcium ion and clays. In the presence calcium and clays, the results would suggest a negative impact on bitumen liberation from sand grains in the industrial process of bitumen extraction from oil sands. In all cases, the contact angle is measured through the bitumen phase.     

生产大颗粒药用磷酸氢钙的探索研究

针对生产药用磷酸氢钙的工艺过程中得率低只有32％,制造成本高、产能低,导致药用大颗粒磷酸氢钙在国内市场供不应求。通过添加颗粒促进剂氢氧化钾将得率提高至66．2％,产能提高一倍,同时生产成本降低1276．4元／吨,大大缓解国内市场供给紧张现状。     

无水磷酸氢钙生产工艺

介绍了一种以液态食品磷酸与碳酸钙及处理后的石灰水(纯净氢氧化钙)反应生产无水磷酸氢钙(牙膏级、药品级、食品级)新工艺。同时提供了按此工艺生产无水磷酸氢钙的生产结果。     

用氯化钙制备高纯超细碳酸钙的研究

以工业生产废渣氯化钙和CO2为主要原料，采用相应的氯化钙溶液精制和CO2净化技术，在碱性氯化钙溶液条件下，喷雾碳化制备高纯超细碳酸钙并副产氯化铵，碳酸钙纯度达99％以上，白度达97％以上，含微量镁、钙、氯，符合精密及电子级陶瓷生产需要，还可用于食品、医药和日化等行业，经济效益及社会效益显著。     

A review of alkali-silica reaction and expansion mechanisms 1. Alkalies in cements and in concrete pore solutions

Current concern with alkali silica reactions is due to rising alkali contents of cements, changed concrete technology, and necessity of employing marginal aggregates in many areas, as well as to new reports of field damage coming to light. A brief overall view of the physicochemical basis for alkali-silica reactions is given. The reaction is primarily one of hydroxide ions rather than of alkali cations; nevertheless the latter are of critical importance. Alkalies in cement are found primarily as alkali sulfates or as solid solution substituents in calcium aluminate or in belite. The rates at which these reach the pore solution phase are discussed, and data indicating that concentrations as high as 0.7 molar may be attained in a month or so and maintained indefinitely are discussed. The relationship between alkali cation concentration and hydroxide ion concentrations are explored, and after a few days of hydration published data indicate that the two are substantially equivalent. Thus reacting pore solutions may have hydroxyl ion concentrations of the order of 0.7 molar, more than 15 times that of pure saturated calcium hydroxide solutions.