氢化诺卜醇及其烷基醚的合成与表征

由β-蒎烯与多聚甲醛反应制得诺卜醇,然后用Ni(R)催化氢化制得氢化诺卜醇(ROH),再将氢化诺卜醇与亚硫酰氯反应制得氢化诺卜基氯(RCl),由RCl分别与6种醇钠反应合成了6种氢化诺卜基烷基醚,各产物的得率均在92%以上,GC纯度95%以上。各产物都用IR,1H NMR,13C NMR与MS进行了结构表征。     

诺蒎酸的超声合成

以β-蒎烯为原料,通过KMnO4氧化辅以超声辐照手段,进行了诺蒎酸的合成条件优化研究.正交实验表明,声强对诺蒎酸的产率影响最大,其次为pH、原料配比、反应温度和时间;单因素实验表明,诺蒎酸的产率随着声强的增大而增大.在声强0.38W/CM2、pH=10、n(β-蒎烯)/n(KMnO4)=1/2、15℃反应30min的优...     

N-二茂铁酰胺酸的合成及反应研究

有机化学中胺与酸酐的反应已有详细、广泛地研究,但在金属有机化学中有关氨基茂金属与酸酐的酰化反应却未见文献报道.为模拟具有生物活性的含有酰胺结构的一类新型金属有机化合物,研究氨基二茂铁与酸酐反应的条件,我们使氨基二茂铁与环二酸酐反应,合成并表征了7种N-二茂铁酰胺酸(A-G),考查它们与金属离子的螯合作用并分离出螯合物H和I.这些配合物(A-I)和酸酐K均未见文献报道.     

TEBA催化合成非诺贝特酸

在50%氢氧化钾溶液中,4-羟基-4'-氯二苯甲酮(1),氯仿和丙酮在相转移催化剂TEBA的催化下发生缩合反应合成了非诺贝特酸.最佳反应条件为:1 30 g,丙酮120 g,TEBA 2.5 g,氯仿40 g,于30 ℃滴加氯仿,产率89.7%.     

超声波辅助提纯氢化枞酸的研究

以氢化松香为原料、乙醇胺为有机胺、乙酸乙酯为溶剂,在超声波辅助下进行胺化反应制备氢化枞酸乙醇胺盐,再经萃取、重结晶和酸化得到氢化枞酸,采用正交试验考察了超声功率、搅拌转速、反应温度、反应时间对氢化枞酸纯度的影响,结果表明,影响氢化枞酸纯度因素按显著程度依次为反应温度>反应时间>超声波功率>搅拌转速,确定了最佳的胺化反应条件为:反应温度40℃、反应时间40min、超声波功率400W、搅拌转速400r/min,所得氢化枞酸的纯度为94.5%。采用GC、GC-MS、FT-IR、熔点仪和旋光仪对氢化枞酸产品进行了分析鉴定。     

聚酯酰胺的合成及表征

用两种方法合成了聚酯酰胺（ＰＥＡ）共聚物．一种是两步法，即先合成对苯二甲酸乙醇酰胺（ＢＡＥＴ）单体，然后与对苯二甲酸乙二酯（ＢＨＥＴ）共缩聚；另一种是一步法．即在酯交换反应中直接添加乙醇胺（ＥＡ）．两种方法制得的聚酯酰胺（ＰＥＡ）共聚物测试证明了为产物，并分析了合成中的化学反应．     

新型去氢枞酸基磺酰胺类化合物的合成及其生物活性

去氢枞酸与SOCl2反应制得去氢枞酸酰氯(2);芳磺酰氯与乙二胺经N-酰化反应制得N-芳磺酰基乙二胺(4a~4k);在DMAP催化下,2分别与4a~4k经N-酰化反应合成了11个新型的去氢枞酸基磺酰胺类化合物(5a~5k),其结构经1H NMR,13C NMR,IR和ESI-MS表征。生物活性测试结果表明,在用药量为50μg·mL-1时,5a~5k对黄瓜枯萎病菌、苹果轮纹病菌、番茄早疫病菌、花生褐斑病菌和小麦赤霉病菌有一定的抑菌活性,其中去氢枞酸基间甲基苯磺酰胺(5c)对番茄早疫病菌的杀菌活性最佳,抑制率为73.6%;在用药量为100μg·mL-1时,大部分化合物对油菜的胚根生长有一定抑制作用,其中去氢枞酸基对甲氧基苯磺酰胺(5d)的抑菌活性最佳,抑菌率为57.1%。     

气相色谱法测定合成产物中诺蒎酸的含量

采用气相色谱法跟踪测定了β-蒎烯氧化反应中主产物诺蒎酸的含量;试验结果表明,在SE-30/Chromosorb W/AW(0.25～0.175 mm)的色谱柱上,诺蒎酸与副产物之间具有较好的分离效果,并且在峰形对称性和出峰时间上,SE-30柱也具有优势;该方法的线性范围在15.0～60.0 g·L-1之间,检出限(S/N=3)为3.5 g·L-1;对同一试样的5次平行测定的相对标准偏差为1.8%;该方法的标准加入回收率达90%～98%.     

不对称芳基取代的方酰胺和异方酰胺的合成

Ｎ－芳基氮氧方酸的活性羟基能够被芳伯胺取代。利用这一特性，可在方酸四碳环上引入另一不同的芳胺基，即可获得不对称芳基取代的方酰胺或异方酰胺。以乙醇等为介质，芳伯胺与７种Ｎ－芳基氮方酸反应，制得２５个不对称的方酰胺和２４个不对称的异方酰胺。该合成方法优点突出，反应简便有效，通用性强。     

Synthesis of fusaric acid and its analogs

Summary 1. A new method for synthesizing fusaric acid and its analogs has been proposed which starts from 2-methyl-5-ethynylpyridine; this is alkylated and the hydrogenated 2-methyl-5-alkynylpyridines are oxidized to the corresponding 5-alkylpicolinic acids.2. The mass-spectroscopic behavior of the 2-methyl-5-alkylpyridines has been studied.Khimiya Prirodnykh Soedinenii, Vol. 3, No. 2, pp. 134–137, 1967     

Synthesis of betulonic acid piperazide and its nitrohetaryl derivatives

Russian Journal of Organic Chemistry -     

Synthesis of quinoline-4-carboxylic acid and its derivatives

2-Methylquinoline-4-carboxylic acid was obtained by the reaction of isatin with acetone in the presence of an alkali. This acid was converted through a step involving (E)-2-styrylquinoline-4-carboxylic acid to quinoline-2,4-dicarboxylic acid, from which quinoline-4-carboxylic acid was obtained by refluxing in nitrobenzene. The structures of the synthesized compounds were confirmed by ¹H NMR spectroscopy using two-dimensional (2DJ) spectra.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 819–821, June, 1988.     

Synthesis and biological activity of RS-abscisic acid and its analogs

Summary RS-Abscisic acid and some of its analogs have been obtained. The biological activity of these compounds has been studied in dependence on their structure.It was found that precursors of RS-abscisic acid suppress the growth of segments of coleoptiles to a considerably smaller extent than the acid itself.Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR. Timiryazev Institute of Plant Physiology. Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 731–735, November–December, 1970.     

Synthesis and biological activity of RS-abscisic acid and its analogs

Chemistry of Natural Compounds - RS-Abscisic acid and some of its analogs have been obtained. The biological activity of these compounds has been studied in dependence on their structure. It was...     

Synthesis of 3-deoxy-3,3-difluoroshikimic acid and its 4-epimer from quinic acid

3-Deoxy-3,3-difluoroshikimic acid 2 and its 4-epimer 3 as new analogues of shikimic acid have been synthesised from quinic acid in overall yields of 30% and 12%, respectively.     

Synthesis of hydrazones of anabasinylacetic acid and structure of its isopropylidenehydrazone

Some hydrazones based on N-anabasinylacetic acid hydrazide have been synthesized. Structure of N′-isopropylidenehydrazone of N-anabasinylacetic acid has been studied by X-ray diffraction.