固体超强酸催化剂对没食子酸月桂醇酯合成收率的影响

目的研究固体超强酸催化剂对没食子酸月桂醇酯合成收率的影响。方法通过改变催化剂焙烧温度、浸渍液浓度及催化剂用量比较没食子酸月桂醇酯合成收率变化,得到最佳反应参数。结果及结论以600℃焙烧3h,以0.5mol.L-1过硫酸铵溶液浸渍的Zr(OH)4制得的催化剂,并在0.01g.mL的浓度下得到酯收率最大。     

超声波辐射合成乙酰水杨酸

乙酰水杨酸又称阿司匹林（Aspirin）,是应用最早、最广泛、最普通的解热镇痛药和抗风湿类药,近年来科学家研究发现,阿司匹林对预防血栓形成有显著作用,更加扩展了其药用价值,成为重要的一类常备药之一。超声波辐射是来开发的新的有机合成方法之一,本文采用超声波辐射的方法对乙酰水杨酸的合成工艺进行了改进。     

固体酸催化合成3-苯甲酰基丙烯酸乙酯的工艺

目的 提高3-苯甲酰基丙烯酸乙酯的产品纯度和总收率.方法 以SO2-4/Si2O2-TiO2复合固体超强酸作为酯化反应催化剂,以苯和顺酐为起始原料,经傅-克、酯化反应制得目标产物,并采用精馏脱水酯化工艺,不断排除酯化过程中的水.结果 酯化毕,用烷基苯转型,产品纯度>98%,总收率≥75%.结论 合成的3-苯甲酰基丙烯酸乙酯,以SO2-4/Si2O2-TiO2复合固体超强酸作为酯化反应的催化剂,可提高产品的纯度和总收率.     

5-硝基水杨酸合成新工艺

目的:采用新方法合成5-硝基水杨酸。方法:以水杨酸为原料,采用硝酸脲/硫酸为硝化试剂,反应得到5-硝基水杨酸以收率为指标考察了反应条件包括硝酸脲/水杨酸物料配比、反应温度、反应时间对反应的影响。结果:得到适合的反应条件为硝酸脲/水杨酸(摩尔比)=1.2:1,反应温度25℃,反应时间6 h,收率为86.4%。结论:新方法收率较高,反应条件温和,适合工业化生产。     

3,5-二碘水杨酸合成的改进

3,5 -二碘水杨酸 ( 1 )是多种农药、兽药和生化试剂的合成中间体。文献[1,2 ] 以冰醋酸或甲醇为溶剂 ,由水杨酸 ( 2 )和氯化碘反应制得 ,此法消耗大量溶剂 ,成本较高 ;另有报道[3 ] 以苯和水做溶剂 ,由 2和70 %双氧水及碘反应制得 ,收率 96% ,但纯度仅90 %。本文直接以水做溶剂 ,加氯化铜为催化剂 (不加催化剂时收率 85 % ,含量 94% ) ,用氯化碘进行碘化制得 ,收率 98% ,纯度 98% ,操作简便 ,成本低 ,是一种较好的工艺路线。反应式如下 :实验部分将 2 ( 1 0 g,0 .0 72 mol)、氯化铜 ( 1 0 g)和水 ( 1 0 0ml)搅拌均匀 ,加热至 5 0℃ ,在 40 m…     

1-乙酰-4-(4-羟基苯基)哌嗪合成的改进

二乙醇胺经溴化、环合一锅合成 N-(4-甲氧苯基)哌嗪氢溴酸盐(3),解决了劳动保护问题。酰化收率经改进从26%提高至70%以上,总收率26.4%,适合工业生产。     

2-乙酰噻吩吖嗪及其过渡金属配合物的合成与活性

目的 研究2-乙酰噻吩吖嗪及其过渡金属Cu^2 ，Fe^3 配合物的合成与生物活性。方法 从2-乙酰噻吩和水合肼出发合成2-乙酰噻吩吖嗪，进而合成了其过渡金属Cu^2 ，Fe^3 的配合物。用MS，^1H—NMR对配体进行了确认。通过元素分析、摩尔电导率、红外光谱、紫外光谱等手段对配合物进行了表征。用NBT法研究了配合物对超氧阴离子自由基的抑制作用；并利用MTT法和SRB法对其进行了抗肿瘤活性体外筛选实验。结果 发现配体和配合物都具有一定的生物活性，且Cu配合物活性较好。结论 配合物的生物活性可能与中心离子的最外层d轨道的电子结构有关。     

乙酰水杨酸－聚－α，β－DL－（2－羟乙基）天冬酰胺共价复合体的合成

本文利用可生物降解的聚－α，β－ＤＬ－（２－羟乙基）天冬酰胺（ＰＨＥＡ）作为高分子载体和乙酰水杨酰氯在吡啶催化下缩合，成为聚天冬酰胺－乙酰水杨酸共价复合体，经用ＮａＯＨ溶液回流全水解后，由高效液相法测得乙酰水杨酸的接入率为３０％（ｗ／ｗ）．文中还对乙酰水杨酰氯的制备方法作了改进，收率为７５．６％。     

2-乙酰氧基-5-乙酰氨基苯甲酸的合成及镇痛抗炎作用

目的　合成2-乙酰氧基-5-乙酰氨基苯甲酸并进行镇痛、抗炎作用的初步研究。方法　以水杨酸和苯胺为原料,经重氮、偶合、还原及酰化合成目标化合物,化学结构经元素分析、IR和¹H-NMR确定;采用小鼠醋酸扭体、耳部肿胀法研究镇痛和抗炎作用。结果　目标化合物的熔点为170～173℃,中和法测含量99.2% ,收率42.7% (以水杨酸计)。小鼠灌胃后抑制醋酸所致疼痛的ED₅₀为1.2mmol/kg ,抑制二甲苯所致耳廓炎症的ED₅₀为2 .3mmol/kg ,LD₅₀为2598mg/kg。结论　2-乙酰氧基-5-乙酰氨基苯甲酸合成简单,收率稳定,具有比阿司匹林和对乙酰氨基酚更强的镇痛和抗炎作用。     

In vitro enantioselective displacement of propranolol from protein binding sites by acetyl salicylic acid and salicylic acid

The influences of acetyl salicylic acid (ASA) and salicylic acid (SA) on the enantioselective binding of propranolol (PL) and its enantiomers to plasma proteins and human serum albumin (HSA) were investigated. The equilibrium dialysis was employed for protein binding studies. We observed statistically significant displacement of racemic-PL, (+)-(R)-PL, and (-)-(S)-PL (0.1-10 microM) from their protein binding sites by ASA (200 microg/ml) and SA (100 microg/ml). ASA and SA displaced PL stereoselectivly from its binding sites. We concluded that ASA and its metabolite SA could change R/S ratio of PL unbound fractions and they might affect pharmacokinetic properties of PL.     

离子色谱法测定烟酸中氯离子和硫酸根离子

目的:建立同时测定烟酸中氯离子和硫酸根离子的离子色谱法。方法:采用阴离子交换色谱,直接电导检测,以2.0 mmol/L邻苯二甲酸和1.9 mmol/L三羟甲基氨基甲烷混合溶液为淋洗液。结果:Cl-和SO42-分别在0.5~200μg/ml(r=0.999 7)和2.0~200μg/ml(r=0.999 7)浓度范围内线性关系良好,烟酸中Cl-和SO42-的方法平均回收率分别为92.7%(RSD为2.99%)和97.5%(RSD为1.98%)。结论:本方法快速、准确,可用于同时检测烟酸中的Cl-和SO42-。     

Comparative pharmacokinetics of acetyl salicylic acid and its metabolites in children suffering from autoimmune diseases

The aim of the present study was to compare the effect produced by juvenile rheumatoid arthritis (JRA) or rheumatic fever (RF) on the pharmacokinetics of acetyl salicylic acid (ASA) and its metabolites in children with autoimmune diseases (AD). METHODS: A prospective, open labelled study was performed in 17 children with JRA and 17 with RF who received a single dose of 25 mg ASA/kg orally. The pharmacokinetics of ASA and its metabolites were determined. The blood and urine levels of each salicylate collected during 24 h were measured by HPLC. A group of 15 healthy teenage volunteers was included as a control group. RESULTS: The maximum plasma concentration, half-life time, area under the curve and the amount of salicylates excreted were statistically different between the JRA and the RF groups, as well as between the RF group and the controls, however, there were no significant differences between the JRA group and the controls. CONCLUSIONS: Dosage schemes must be adjusted for JRA patients, since the half life in these patients is longer than in RF patients. However, due to ample variability of pharmacokinetic parameters it is recommended that dose schemes are individualized on the type of autoimmune disease considered.     

Flow-through UV spectrophotometric sensor for determination of (acetyl)salicylic acid in pharmaceutical preparations

The solid phase spectrophotometry technique, in which the absorbance of the species of interest sorbed on a solid support is measured directly, was applied to the determination of salicylic acid using flow injection-analysis. Salicylic acid was determined by monitoring of its intrinsic absorbance at 297 nm sorbed on Sephadex QAE A-25 resin placed in an appropriate flow-through cell. The method proposed improves the selectivity compared with the corresponding solution-phase method and the sensitivity is increased by a factor of 30 or more. The flow-through sensor proposed allows working with several calibration lines simply by varying the sample volume injected. Thus, linear dynamic ranges from 1 to 20 and from 2 to 40 microg ml(-1) can be obtained by using 1000 and 300 microl, respectively, with detection limits being 0.064 and 0.135 microg ml(-1). Relative Standard Deviations (RSDs) of 0.52 and 0.38%, and sampling frequencies of 18 and 25 h(-1), respectively, were also achieved. The sensor also allows the indirect determination of acetylsalicylic acid previous hydrolysis on-line to salicylic acid. For acetylsalicylic acid, a linear dynamic range from 5 to 120 microg ml(-1) and 25 h(-1) of sampling frequency (300 microl of sample volume) were obtained. The proposed flow-through sensor has been successfully applied to the determination of both analytes in pharmaceutical preparations.     

Synthesis and antipyretic activity of new salicylic acid derivatives

New salicylic acid derivatives were synthesized. Their antipyretic activity and acute toxicity were studied. Translated from Khimiko-Farmatsevticheskii Zhurnal, Vol. 42, No. 10, pp. 24–26, October, 2008.