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以5-氨基-2-巯基-1,3,4-噻二唑为原料,经过胺基酰基化、氯气氧化制得5-乙酰胺基-1,3,4-噻二唑-2-磺酰氯,化合物与N-甲基哌嗪、苯胺反应,合成两个未见报道的目标产物:5-乙酰胺基-1,3,4-噻二唑-2-(N-甲基哌嗪磺酰胺)和5-乙酰胺基-1,3,4-噻二唑-2-(磺酰苯胺).利用IR、H-NMR、LC-MS对目标产物进行表征. 相似文献
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本文研究了使用带水剂分水促进N-烷基化反应合成N,N-二甲氧基羰基甲基取代苯胺类染料中间体的新工艺。以间氨基乙酰苯胺(或2-氨基-4-乙酰氨基苯甲醚,统称取代苯胺)和氯乙酸甲酯为原料,碳酸钠为缚酸剂,溴化钠为催化剂,采用带水剂合成3-乙酰氨基-N,N-二甲氧基羰基甲基苯胺(或2-甲氧基-5-乙酰氨基-N,N-二甲氧基羰基甲基苯胺)。确定其最佳工艺条件为:n(碳酸钠)∶n(取代苯胺)=1.2∶1,催化剂溴化钠量为取代苯胺(质量分数)的10%,0.5 mol取代苯胺投料,取100g甲苯作为带水剂,回收带水剂(含氯乙酸甲酯)可用于下批合成(即套用)。 相似文献
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田华 《精细与专用化学品》2012,20(5):27-29,45
以1,5-二氨基葸醌为原料,与苯甲酰氯反应,以苯甲酸甲酯为溶剂,以碳酸钠作缚酸剂,制得1-氨基-5-苯甲酰氨基蒽醌,并对合成工艺进行了优化。优化条件为:n(苯甲酰氯):n(1,5-二氨基蒽醌)=1.4:1,反应温度140℃,保温2h。在此条件下,目标产物收率比原工艺提高13%。采用熔点测定、红外光谱(IR)、液相色谱(HLPC)进行分析和结构表征。 相似文献
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杂多酸(盐)催化合成肉桂酸异戊酯的研究 总被引:11,自引:0,他引:11
以杂多酸(盐)为催化剂,3A分子筛为脱水剂,肉桂酸和异戊醇为原料合成肉桂酸异戊酯,考察了醇酸比、催化剂种类、催化剂用量、反应时间对酯产率的影响。结果表明,在肉桂酸用量为01mol情况下,用AlPW12O40为催化剂,催化剂用量为100g,醇酸摩尔比为25∶1,反应时间3h,反应温度135~140℃是最适宜的反应条件。酯产率超过96%。 相似文献
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Acrylic type polymeric systems having degradable ester bonds linked to 5-aminosalicylic acid were synthesized and evaluated
as materials for drug delivery. 5-Aminosalicylic acid, as an important drug in the treatment of inflammatory bowel diseases,
was linked to 2-hydroxyethyl methacrylate by activated ester methodology in two-step and one-pot procedures to obtain methacryloyloxyethyl
5-amino salicylate. The resulting methacrylic derivative of 5-aminosalicylic acid was copolymerized with methacrylamide, 2-hydroxyethyl
methacrylate and methyl methacrylate (in 1:3 mole ratio) by free radical polymerization method in N,N-dimethylformamide solution, utilizing α,ά-azoisobutyronitrile as initiator at the temperature range of 65–70 °C. The obtained
polymers were characterized by FT-IR, 1H NMR, 13C NMR and elemental analysis. The average molecular weights of the polymers bearing drug units as side substituents of the
acrylic backbone were determined by gel permeation chromatography and their polydispersity indices resulted in the range of
1.6–1.8. Release studies of 5-aminosalicylic acid were performed into dialysis bags by hydrolysis in buffered solutions (pH
1, 7 and 8) at 37 °C. Detection of hydrolysis by UV spectroscopy at selected intervals showed that the drug can be released
by selective hydrolysis of the ester bond at the side of drug moiety. The release profiles indicated that the hydrolytic behavior
of polymeric prodrugs is strongly based on the polymer hydrophilicity and the pH value of the hydrolysis solution. The results
suggest that these systems could be useful for preparation of a controlled release formulation of 5-aminosalicylic acid in
colon. 相似文献
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The development of a pH sensitive, biodegradable polymer from the combination of Shellac (a natural polymer secreted by lac insect) and polyamidoamine (PAA) (a synthetic polymer) yielded a new biocompatible polymer Shellac-PAA in a photopolymerization process. Scanning electron micrograph of Shellac-PAA shows an interesting heterogeneous surface morphology supported with observation of two different melting temperatures obtained from differential scanning calorimetric measurement. The equilibrium swelling properties of the polymeric material was studied as a function of pH and time in buffer solutions similar to that of gastric and intestinal fluids. The controlled release kinetics of a model colon specific drug 5-aminosalicylic acid showed Fickian diffusion behavior. The new polymer is biocompatible, biodegradable and, hence, projected as a new kind of polymer with improved properties, which can be a potential candidate for controlled release of therapeutic agents in colon specific diseases. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012 相似文献
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采用RP-HPLC测定美沙拉嗪肠溶片中5-氨基水杨酸(5-ASA)的含量。柱前衍生化使样品中5-ASA乙酰化,采用反相高效液相色谱法,色谱柱为ODS C18,流动相为磷酸盐缓冲液-乙腈(92∶8),流速为0.9 m L·min-1,检测波长为304 nm。结果表明,5-ASA在3.12~50.0μg·m L-1范围内线性关系良好(r=0.999 6),平均回收率为100.8%,RSD为1.27%,柱前衍生化高效液相色谱法测定美沙拉嗪肠溶片中5-ASA的含量简便、快速、准确、专属性强,适用于美沙拉嗪肠溶片中5-ASA的含量测定。 相似文献
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G. Usha RANI Kartick Prasad DEY Srijita BHARTI Sumit MISHRA 《Frontiers of Chemical Science and Engineering》2014,8(4):465
The utilization of poly (2-hydroxyethylmethacrylate) grafted agar (Ag-g-P(HEMA)) as a matrix for the controlled release of 5-aminosalicylic acid was investigated. Grafted copolymers of 2-hydroxyethylmethacrylate (HEMA) monomers on agar were synthesized by microwave assisted method. In vitro drug release studies were performed at pH values of 2 and 7 in order to investigate the possibility of pH triggered release for colon targeted drug delivery. Further, the percent grafting vs. t50 (the time taken for release of 50% of the enclosed drug) value was studied and the results indicate that it may be possible to develop a programmable drug release matrix based on grafted polysaccharide. Ag-g-P(HEMA) appears to be a useful matrix for controlled release. 相似文献
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Dianyu Yu Xu Wang Dan Li Xin Zhang Changhua Yu Xingwu Pei Jinju Cheng Liqi Wang 《European Journal of Lipid Science and Technology》2020,122(4)
Oil sources (canola, sunflower, and flax‐seed oil) characterized by unsaturated fatty acids are gelled by using cinnamic acid. The physical characteristics and crystallization kinetics of cinnamic acid‐based organogels are investigated. A phase diagram with cinnamic acid concentrations ranging from 1% to 7% (w/w) shows that both canola and sunflower oil organogels are formed at 3.0% (w/w) cinnamic acid at 5 °C. The flax‐seed oil organogels are formed at 4.0% (w/w) at 5 °C. Firmness is shown to be dependent on the fatty acid composition and viscosity of the oil. Flax‐seed oil with a higher degree of unsaturation and lower viscosity tends to produce harder organogels. This result is consistent with the observations of polarized light microscopy. The organogels have low solid fat content at 35 °C which is close to the human body temperature, and no effect of oil type is found. The X‐ray diffraction measurements show β'‐form crystal exists in three types of organogels. The thermal properties vary in different types of organogels. The crystallization kinetics results suggest that three types of organogels crystallize by 1D and 2D mixed growth and instantaneous nucleation. Practical Applications: These findings provide in‐depth characteristics of cinnamic acid‐based organogels, which are a substitute for solid fats. 相似文献