5-氟-2-溴苯甲酸的制备实验研究

以乙酸为溶剂 ,乙酸钴、乙酸锰、溴化钠为催化剂 ,由氧气在常压下氧化 5 -氟 - 2 -溴甲苯制备 5 -氟 - 2 -溴苯甲酸 ,反应温度 12 0～ 130℃ ,反应物质量分数为 16 .8%～ 2 0 .2 % ,催化剂用量为原料的 2 .5 %～ 4 %时 ,收率较高     

2-(对-氯苯基)-5-三氟甲基吡咯-3-腈的合成

以对氯苯甘氨酸为原料，在催化剂的作用下生成4-(对-氯苯基)-2-三氟甲基-3-恶唑-5酮，再在碱性条件下生成2-(对-氯苯基)-5-三氟甲基吡咯-3-腈，收率为86．1％，纯度达97％以上。此操作简便，反应条件比较温和，对环境的污染较小，适合于工业化生产。     

5-溴-2-氟苯磺酰氯的合成研究

5-溴-2-氟苯磺酰氯是一种重要的有机合成中间体,被广泛用于农药、染料、医药等的合成过程中。文章以市场上易得的5-溴-2-氟苯胺为原料,经重氮化、氯磺酰化合成目标产物,产物结构经MS和1HNMR进行表征,收率为86.5%。该合成工艺具有成本低、反应选择性好、条件稳定、收率高、后处理简单等优点。     

光催化氧化合成2-氟-3-硝基苯甲酸的研究

以2-氟-3-硝基甲苯为原料、醋酸为溶剂、硫酸铜和氢溴酸为催化剂,经光催化氧化合成新型杀虫剂溴虫氟苯双酰胺和环丙氟虫胺的关键中间体2-氟-3-硝基苯甲酸.含量98％,收率90.0％,反应条件温和,工艺环保,具有较高的应用价值.     

3-溴-5-氟苯甲腈的合成

以2-氨基-5-氟苯甲酸为原料,经溴代、重氮化、还原合成中间体3-溴-5-氟苯甲酸,再以甲苯为溶剂,氯化亚砜氯化后通入氨气,所得酰胺和五氧化二磷共热蒸馏得标题化合物,总收率53.4%(以2-氨基-5-氟苯甲酸计)。     

2-氟-5-溴硝基苯的合成

采用冰醋酸作为溶剂,以邻氟硝基苯为原料,N-溴代丁二酰亚胺(NBS)为溴代试剂,合成了2-氟-5-溴硝基苯。所得目标产物通过GC-MS定性、GC定量检测。结果表明,最佳反应条件为:n(邻氟硝基苯)∶n(NBS)=1∶1.05,以冰醋酸作溶剂,反应温度10℃,反应时间2 h,在该条件下2-氟-5-溴硝基苯的收率为98.6%,原料转化率100%。该反应条件温和,易于控制,重复性好。     

2-溴-3-{4-[2-(5-乙基-2-吡啶基)-乙氧基]苯基}丙烯酸甲酯的合成

以5－乙基－2吡啶基乙醇为起始原料,与对氟硝基苯缩合,Pd/C催化加氢,得4－[2－（5－乙基－2－吡啶基）－乙氧基]苯胺,再经重氮化和桑德迈尔反应,制得2－溴－3－{4－[2－（5－乙基－2－吡啶基）－乙氧基]苯基}丙烯酸甲酯,总收率为65．6％,最终产物经IR和NMR结构确证。     

5-氟烟酸的合成

以烟酸(Ⅰ)为原料,经3步反应合成5 氟烟酸(Ⅵ)。Ⅰ与SOCl2在50℃回流4h后,除去SOCl2,170℃溴化12h,水解得5 溴烟酸(Ⅲ),收率为91%;Ⅲ于反应釜中,Cu2+为催化剂,与氨水在190℃反应24h,氨化得5 氨基烟酸(Ⅳ),收率为75%;Ⅳ应用希曼反应,在0℃重氮化,HBF4氟代得氟硼酸盐(Ⅴ),70℃热解Ⅴ得Ⅵ,收率77%。5 氟烟酸结构经FTIR、GC-MS证实。     

一种可工业化的2-溴-5-氟三氟甲苯的制备方法

以邻三氟甲基苯胺为原料,经桑德迈尔反应溴代、硝化、加氢还原,最后再重氮化氟代合成2-溴-5-氟三氟甲苯,总收率70%;该方法原料廉价易得,所涉及到的反应都是工业上较成熟的反应,可工业化生产。     

3-(2-氟-4-氯-5-甲氧羰基乙巯基苯基)-5-异丙叉基恶唑烷-2,4-二酮的合成

通过2-氟-4氯-5甲氧羰基乙巯基苯基异氰酸酯与2—羟基—3—甲基—3—丁烯酸乙酯发生加成、闭环反应制得除草剂3—(2—氟-4氯—5—甲氧羰基乙巯基苯基)—5-异丙叉基噁唑烷—2，4-二酮，优化反应条件为n(异氰酸酯)：n(2—羟基—3—甲基—3—丁烯酸乙酯)＝1：1．25—1：1．30。     

Strategies for introducing sulfur atom in a sugar ring: synthesis of 5-thioaldopyranoses and their NMR data

Thiosugars containing a sulfur atom as heteroatom in the sugar ring are highly interesting. In particular, 5-thioaldopyranoses have attracted considerable attention because they exhibit biologically important properties as the substrates for glycosidases also can be developed as potential therapeutical agents, such as antineoplastic, anti-diabetic, antiviral, and antithrombotic agents. In this review, we describe and discuss the advances in synthetic strategies for the preparation of 5-thioaldopyranoses (5-thio-d-hexoses, 5-thio-l-hexoses, 5-thio-d-pentoses and 5-thio-l-pentoses), as well as their spectroscopic NMR data as known to date. The study aims to give readers an easy understanding of thiosugars chemistry and provide a useful guide for carbohydrate chemists.     

无致癌诱变性二元胺的直接染料

综述了用2,2'-二甲基-5,5'-二丙氧基联苯胺和5,5’-二丙氧基联苯胺作为重氮组分的直接染料的合成和检测。TLC检测染料的纯度,其最大可见吸收为485-601nm,摩尔消光系数为2.2×104-6.4×104L/mol.cm,用ESMS确定染料的化学结构。这类直接染料无致癌诱变性,并具有良好的应用和牢度性能。有20篇参考文献。     

N-乙酰-5-甲氧基色胺的工艺研究进展

综述了N-乙酰-5-甲氧基色胺主要的合成方法,并对各路线的优缺点进行评价,提出了可行的改进方向.     

呈味核苷酸二钠结晶工艺研究

呈昧核苷酸二钠包括5’-肌苷酸二钠和5’-鸟苷酸二钠，难以形成良好的结晶体，针对现有研究中存在的问题。对呈味核苷酸二钠结晶工艺进行改进，优化工艺参数。研究发现，采用乙醇为溶析剂，在合适的结晶液浓度和溶析剂添加量的条件下，添加晶种程序降温结晶，有利于提高结晶收率、产品纯度和堆密度。在优化的结晶条件下，呈味核苷酸二钠产品色谱纯度达到99．54％，堆密度达到0．54g/cm3，满足国际市场的要求。     

一锅法合成N_4-乙酰-5-氟胞苷的新工艺研究

介绍了合成N4-乙酰氟胞苷的新工艺。在溶剂中5-氟胞嘧啶∶六甲基二硅胺烷(HMDS)∶三甲基氯硅烷(TMCS)∶四乙酰核糖(摩尔比)=1∶0.8∶0.8∶1,以无水四氯化锡为催化剂,一锅法合成5-氟胞苷,并以甲醇为溶剂直接用乙酐酰化得到N4-乙酰氟胞苷。总收率77%以上。     

LPPR5 Expression in Glioma Affects Growth,Vascular Architecture,and Sunitinib Resistance

Despite intensive research, glioblastoma remains almost invariably fatal. Various promising drugs targeting specific aspects of glioma biology, in addition to or as an alternative to antiproliferative chemotherapy, were not successful in larger clinical trials. Further insights into the biology of glioma and the mechanisms behind the evasive-adaptive response to targeted therapies is needed to help identify new therapeutic targets, prognostics, or predictive biomarkers. As a modulator of the canonically oncogenic Rho-GTPase pathway, Lipid phosphate phosphatase-related protein type 5 (LPPR5) is pivotal in influencing growth, angiogenesis, and therapeutic resistance. We used a GL261 murine orthotopic allograft glioma model to quantify the tumor growth and to obtain tissue for histological and molecular analysis. Epicortical intravital epi-illumination fluorescence video microscopy of the tumor cell spheroids was used to characterize the neovascular architecture and hemodynamics. GL261-glioma growth was delayed and decelerated after LPPR5 overexpression (LPPR5^OE). We observed increased tumor cell apoptosis and decreased expression and secretion of vascular endothelial growth factor A in LPPR5^OE glioma. Hence, an altered micro-angioarchitecture consisting of dysfunctional small blood vessels was discovered in the LPPR5^OE tumors. Sunitinib therapy eliminated these vessels but had no effect on tumor growth or apoptosis. In general, LPPR5 overexpression generated a more benign, proapoptotic glioma phenotype with delayed growth and a dysfunctional vascular architecture.     

Meadowfoam fatty amides: Preparation,purification, and use in enrichment of 5,13-docosadienoic acid and 5-eicosenoic acid

Recrystallization from hexane of amides prepared from meadowfoam fatty acids provides crystals of the monoenoic fatty amides. Hydrolysis of the crystals, or the mother liquor, provides meadowfoam fatty acids that are enriched in 5-eicosenoic acid and 5,13-docosadienoic acid, respectively. The meadowfoam fatty amides may be useful as slip and antiblock agents in polyolefin film.     

2，5-二氨基甲苯系列产品合成技术的研究与进展

在系统介绍2,5-二氨基甲苯基本合成方法的基础上,以经济、环保和新型工业化作要求,重点评述了各种方法的工艺特点、研究中的技术进展以及实施商品化生产的可行性。结果表明,以邻甲苯胺为原料经重氮偶合、还原氢解是合成2,5-二氨基甲苯及其系列产品优先的技术路线。同时提出了高质量、低成本、清洁化发展该系列产品的研究方向和内容建议。     

Dehydrogenation and aromatization of methane under non-oxidizing conditions

The dehydrogenation and aromatization of methane on modified ZSM-5 zeolite catalysts has been studied under non-oxidizing conditions with a fixed bed continuous-flow reactor and with a temperature programmed reactor. The results show that benzene is the only hydrocarbon product of the catalytic conversion of methane at high temperature (973 K). The catalytic activity of ZSM-5 is greatly improved by incorporating a metal cation (Mo or Zn). H₂ and ethene have been directly detected in the products with a mass spectrometer during TPAR. A carbenium ion mechanism for the activation of methane is suggested.