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4-(5-硝基-6-羟基-2-苯并(噁)唑基)苯甲酸甲酯的合成 总被引:1,自引:0,他引:1
研究了以关键中间体4-氨基-6-硝基间苯二酚盐酸盐(ANR·HCl)和对苯二甲酸单甲酯(MTA)为原料,分别经酰氯化、缩合、环合分步或原位合成AB型新单体前体-4-(5-硝基-6-羟基-2-苯并唑基)苯甲酸甲酯(MNB)的技术. 反应优化条件为:在甲基异丁基酮溶剂中,n(ANR·HCl)∶ n(MTA)=1.00∶ 1.03,115 ℃缩合反应2.5 h,m(ANR·HCl)∶ m(PPA)=1.00∶ 3.25的多聚磷酸(PPA),120 ℃环合8.5 h,MNB收率75.68%(以ANR·HCl计),HPLC测定ω(MNB)=96.32%. 产物结构经1H NMR和IR测试技术得以确证. 相似文献
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以2-氨基-4-甲氧基苯甲酸甲酯为原料,通过氯代反应,再分别通过酯水解反应得到化合物2-氨基-5-氯-4-甲氧基苯甲酸和2-氨基-3-氯-4-甲氧基苯甲酸。其中间体及产物结构经~1H NMR、~(13)C NMR和ESI-MS确证,并考察了最佳氯代反应条件。结果表明:物料配比为n(2-氨基-4-甲氧基苯甲酸甲酯)∶n(NCS)=1∶1. 2,反应溶剂为N,N-二甲基甲酰胺,反应时间为16 h,两种氯代产物2-氨基-5-氯-4-甲氧基苯甲酸甲酯和2-氨基-3-氯-4-甲氧基苯甲酸甲酯收率分别为47%和39%。 相似文献
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以3,4-二羟基-2,5-呋喃二甲酸或其二甲酯为原料,与手性氨基醇直接缩合,经一步反应合成了3个3,4-二羟基-2,5-双-[2-′(4-′-取代唑啉)]呋喃化合物,产率为90%~94%,其结构经1H NMR谱、IR谱、MS谱和元素分析测试技术得到确证;并应用这些手性双唑啉配体,初步探讨了β-萘乙酮在KBH4或NaBH4作用下的不对称还原反应。结果表明,以环己烷作溶剂,采用n(配体)∶n(还原剂)∶n(β-萘乙酮)=0.04∶1.6∶1在0℃下反应72 h,产物的ee值高达83.2%,且唑啉环上4位取代基为苄基的呋喃类双唑啉,其对映选择性优于取代基为乙基的同类配体。 相似文献
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以4,6-二氨基间苯二酚二磷酸盐和对氨基苯甲酸为原料,在多聚磷酸中,添加还原剂SnCl_2·2H_2O,经缩聚反应合成了有机二胺单体——2,6-二(对氨基苯)苯并[1,2-d;5,4-d']二噁唑(DIABO),其结构经~1H NMR和FT-IR确证。最佳反应条件为:1 0.01 mol,PPA中P_2O_5质量分数为84%,SnCl_2·2H_2O用量为8 wt%,在氮气保护下于200℃反应4 h,产率97%。TG研究结果表明:DIABO的起始分解温度为401.0℃。 相似文献
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Synthesis of cyclic oligo(ethylene adipate)s and their melt polymerization to poly(ethylene adipate)
We present here the first synthesis of cyclic oligo(ethylene adipate)s(COEAs) via pseudo-high dilution condensation reaction of adipoyl chloride with ethylene glycol, and the synthesis of corresponding poly(ethylene adipate)(PEA) via the melt polymerization of COEAs. The structure of COEAs was characterized and proved by 1H-NMR and MALDI-TOF mass measurements. The effects of organic base, reaction temperature and the ratio of adipoyl chloride to ethylene glycol on the yield of COEAs were studied, and the optimum reaction condition was revealed. PEA, a diacid and diol based semi-crystalline green aliphatic polyester, was synthesized by the melt polymerization of COEAs using Ti(n-C4H9O)4 as catalyst and 1,10-decanediol as initiator at 200 °C, which follows the polycondensation-coupling ringopening polymerization method. Our strategy should be applicable to the synthesis of versatile aliphatic polyesters based on diacid and diol monomers, which have potential applications as biocompatible and biodegradable materials. 相似文献
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七十年代初期美国Mobil公司首先研究成功的ZSM-5沸石分子筛,由于它具有独特的孔道结构,对烷基化,异构化,选择裂化和甲醇合成汽油等反应具有独特的催化性能,目前已成为被普遍重视的新型催化剂材料[1-4]。 相似文献
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N-硬脂酰基亮氨酸的合成 总被引:3,自引:0,他引:3
采用酰氯化反应与缩合反应两步法合成N -硬脂酰基亮氨酸。以硬脂酸和亚硫酰氯为原料 ,n(硬脂酸 )∶n(亚硫酰氯 ) =1∶1 .5 ,在 80℃下冷凝回流 6h酰氯化反应合成硬脂酰氯 ,硬脂酰氯经减压蒸馏收集 1 70~2 0 0℃的馏分得到。硬脂酰氯收率为 65 %。硬脂酰氯再与亮氨酸的氢氧化钠溶液在冰水浴中进行Schotten -Baumann缩合反应制得N -硬脂酰基亮氨酸。缩合反应最佳工艺条件是反应溶液pH值控制为 9.0。反应后滴加1mol/L盐酸至pH =5 .0~ 6.0 ,加入正己烷使N -硬脂酰基亮氨酸处于水层中 ,分离并蒸干水层溶液得含NaCl的混合物。用无水乙醇萃取混合物 ,萃取液蒸干得产物。N -硬脂酰基亮氨酸收率为 75 % 相似文献
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以2,4-二氯-6-苯基-1,3,5-三嗪为原料,通过傅克和氧化反应制备了一种新型芳香二酸2,4-二(4-甲酸基苯基)-6-芳基-1,3,5-三嗪(PTDA),并采用1H-NMR,FTIR,MS和元素分析等对其结构进行了表征.利用正交试验,重点考察了氧化反应条件对产率的影响,结果表明反应温度为25℃、反应时间为8 h、HAc与H2SO4摩尔比为10∶1、CrO3与PTDA配比为4∶1时,氧化产率最高,达81.3%.以PTDA和间苯二胺(BD)为原料,制备了新型含1,3,5-三嗪聚芳酰胺PPA,其特性黏数为0.49 dL/g.该聚酰胺表现出较好的溶解性能以及优异的热稳定性和机械性能,室温下可溶于N-甲基-2-吡咯烷酮、N,N-二甲基乙酰胺等溶剂中,由其溶液可制得透明薄膜;玻璃化转变温度达315℃,氮气中起始分解温度T5%为493℃,700℃下残炭率高达59%;薄膜的拉伸强度为82 MPa,断裂伸长率在8.2%,起始模量为2.3 GPa. 相似文献
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H. S. Patel H. J. Mistry 《Phosphorus, sulfur, and silicon and the related elements》2013,188(6):1085-1093
4-(4′-sulphanilyl)-1-phenyl pipearzine (2) has been prepared by ther reaction of N-acetyl sulphanilyl chloride (ASC) with 1-phenyl piperazine followed by the hydrolysis of the product by ethanolic HCl. The hydrolyze product on facile condensation reaction with aromatic aldehydes yields Schiff bases/anils/azomethines (3a–h). These anils on cyclo condensation reaction with chloro acetyl chloride and thio glycolic acid (mercapto acetic acid) yields 2-azetidinones and 4-thiazolidinones respectively. Biological screening of the prepared compounds have been screened on some strains of bacteria. 相似文献
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Cationic polymer as a kind of flocculant is widely applied in purification treatment of waste water. Because it has positive charge group, it is able to connect strongly the suspended matters, short cellulose and other microparticles. The research on synthesis of cationic polymer and application in treatment of waste water is very universal abroad. But domestic research on those is not general. The technology of synthesis of PEM is simple, and the production cost is low. It is easy to apply in treatment of waste water.Synthesis of PEM Emulsion FlocculantSome distilled water, PVA(poly(vinyl alcohol)), EA(ethyl acrylate), and K2S2O8(potassium persulfate) were put into reaction vessel. Kept stirring up under nitrogen. When heated the solution to 40℃, dropped the water solution of MTA[(2-methacryloxylethyl)trimethyl ammonium].Maintained the temperature at 70℃, reacted about 7-8 hours. Then got the PEM emulsion. Changed the ratio of EA and MTA. Obtained a series of PEM emulsions.Stability and Convertibility of PEM EmulsionThe test results showed that when the EA/MTA was 85/15, the PEM emulsion was most stable.When the total monomer quantity was 35%, the convertibility of PEM emulsion was the highest,i.e.98.6%.The MTA Copolymerization Ratio and Morphology of PEM EmulsionWhen the monomers EA/MTA=85/15 and total monomer quantity was 35%, the MTA copolymerization ratio of PEM emulsion was 95.15%(the highest), and the PEM emulsion was some microspheres with 100-180nm of diameter.The Test Results of PEM Emulsion in Treatment of Waste Water The PEM emulsion flocculant was applied in treatment of waste water of paper mill, and measured the precipitation time(t) and transmittancy(T). The test results were showed in table 1. The optimum value of PEM which was able to make the waste water of paper mill into clear water was 0.008%. 相似文献
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以硝基乙烷为原料, 经缩合、 氧化及酯化反应, 设计合成了含能增塑剂2,2-偕二硝基丙基三氟丙酸酯(DNPTFP); 利用核磁共振波谱、 红外光谱和元素分析对其结构进行了表征. 优化了DNPTFP的合成工艺, 确定酯化反应的较佳反应条件: 以甲苯为反应溶剂, n(2,2-偕二硝基丙醇)∶n(三氟丙酸)=1∶1.10, 催化剂浓硫酸的质量分数为5.0%, 反应温度110 ℃, 反应时间10 h. 在此条件下, DNPTFP的收率和纯度分别为75.2%和99.0%. 热分析测试结果表明, DNPTFP的玻璃化转变温度为-80.5 ℃, 热分解温度为267.59 ℃; 机械感度测试结果表明, DNPTFP的撞击感度为H50=125.9 cm, 摩擦感度为0, 说明DNPTFP具有良好的低温性能、 热稳定性及较低的机械感度. 此外, 相溶性试验、 黏度及玻璃化转变温度测试结果表明, DNPTFP与聚叠氮缩水甘油醚(GAP)相溶性良好, DNPTFP可显著调控GAP的黏度和玻璃化转变温度, 并且随其含量增加黏流活化能逐步降低, 增塑效率逐步升高. 因此, DNPTFP对GAP展现出优良的增塑效果, 在GAP基火炸药配方中有良好的应用前景. 相似文献