2-苄硫基-3-吡啶甲酸的合成及应用

评述了2-苄硫基-3-吡啶甲酸的主要合成方法,并对其主要用途进行了介绍.     

3-吡啶甲酸酯类衍生物的合成及卷烟加香应用研究

为了开发新型烟用香料,将烟酸与各种香味醇合成3-吡啶甲酸酯添加到卷烟中,并对其卷烟加香效果进行评价。以3-吡啶甲酸和一系列具有香味的醇为原料,经酰氯化反应先制成3-吡啶甲酰氯,再与香味醇回流反应生成3-吡啶甲酸酯类衍生物。所有化合物结构均经1 H NMR、13^ C NMR、IR和HRMS得到确证。对目标产物进行卷烟加香评吸,评吸结果表明,与对照卷烟相比,加入各种3-吡啶甲酸酯类衍生物的卷烟香气质改善,香气量增加,达到烟香协调、余味净化、杂气减轻的效果。合成的新型吡啶酯类衍生物将有可能作为香原料应用到卷烟中。     

7-羟甲基咪唑并[1,2-a]吡啶的合成

以6-氨基-3-吡啶甲酸为起始原料,经过酯化反应、环合反应、还原反应得到7-羟甲基咪唑并[1,2-a]吡啶,总收率为42％.     

合成8-氯-10，11-二氢-4-氮杂-5H-二苯并[a，d]-5-环庚酮研究进展

介绍了氯雷他定的重要中间体8-氯-10,11-二氢-4-氮杂-5H-二苯并[a,d]-5-环庚酮的基本性质和用途,叙述了以2-溴-3-甲基吡啶、2-[（叔丁基氨基）]-3-甲基吡啶、3-甲基吡啶甲酸和3-吡啶甲酸乙酯为原料出发的合成方法。     

2- 氯烟酸的合成及应用

2-氯烟酸又名2-氯尼古丁酸，化学名称为2-氯-3-吡啶甲酸，由于其特殊的生理活性，广泛用作农药和医药的中间体，可生产农用除草剂、杀虫剂、医用抗菌素等。     

3—吡啶甲酸的合成与应用

3-吡啶甲酸是重要的医药中间体，我国目前生产能力约2000t/a，近年来市场需求量迅速上升，供需矛盾十分突出。预计2005年我国饲料工业3-吡啶甲酸需求量将达2500t，医药工业将达600t。本详细介绍了该产品的生产工艺、生产现状以及用途和市场需求等。     

一种4-氟-3-甲基-2-吡啶甲酸甲酯的制备方法

正本发明公开了一种4-氟-3-甲基-2-吡啶甲酸甲酯的制备方法,属于六元含氮杂环化合物的合成技术领域。本发明的技术方案要点包括3-甲基-2-吡啶甲酸甲酯的合成、3-甲基-2-吡啶甲酸甲酯N-氧化物的合成、4-硝基-3-甲基-2-吡啶甲酸甲酯N-氧化物的合成、4-氨基-3-甲基-2-吡啶甲酸甲酯的合成和目标产物4-氟-3-甲基-2-吡啶甲酸甲酯的合成。本发明利用一步反应合成3-甲基-2-吡啶甲酸甲酯进一步合成4-氟-3-甲基-2-吡啶甲酸甲酯,缩短了工艺流程,且原料廉价易得,反     

2-溴-6-甲基吡啶甲酸甲酯的合成工艺研究

2-溴-6-甲基吡啶甲酸甲酯是一种重要的医药、农药中间体,在抗癌和抗炎方面都有重要用途。对2-溴-6-甲基吡啶甲酸甲酯的合成工艺进行了研究,以3-氰基-6-甲基-2(1H)-吡啶酮为起始原料,经过溴代、水解、酯化三步反应得到目标化合物,其结构经¹H-NMR和MS表征。该合成路线具有原料成本低廉易得、反应条件较温和、后处理简单、收率高等优点,总收率达87.60%,适合工业化生产。     

N,N′-二(2-吡啶甲酰胺基)-1,2-乙烷的合成

以2-吡啶甲酸与乙二胺为原料,采用亚磷酸三苯酯法合成N,N′-二(2-吡啶甲酰胺基)-1,2-乙烷。实验结果表明优化的反应条件为:反应温度90°C,反应时间3 h,n(亚磷酸三苯酯)∶n(2-吡啶甲酸)=0.7∶1,收率为85.6%。产品经HPLC分析,含量99.2%。化合物结构经MS、IR、1H NMR确证。亚磷酸三苯酯法具有操作简便、所得产品纯度高等特点。     

1,2-二(2-吡啶甲酰胺基)苯的合成

以2-吡啶甲酸与邻苯二胺为原料,分别采用两种不同的方法合成了标题化合物.研究表明,亚磷酸三苯酯法具有操作简便、所得产品纯度高等特点.通过正交试验优化的反应条件为:反应温度120℃,反应时间3 h,n(亚磷酸三苯酯):n(2-吡啶甲酸)=0.67:1,收率为82.5%.产品经HPLC分析,含量99.7%.化合物结构经MS、IR、1HNMR确证.     

Untersuchungen zum Verlauf der Cyclisierung von Alkylmalonsäure- und β-Amino-crotonsäureestern zu alkylierten Hydroxypyridincarbonsäureestern

Investigations on the Cyclization of Alkylmalonic Acid Esters with β-Aminocrotonic Acid Esters to Alkylated Hydroxypyridine Carboxylic Acid Esters The cyclization of substituted malonic esters with β-aminocrotonic acid alkyl esters yields 2,4- or 4,6-dihydroxy-3-pyridinecarboxylic acid esters, respectively, in dependence on the reaction conditions and the nature of the substituent in the malonic esters. In the presence of alcoholate malonic acid alkyl esters and alkylmalonic acid alkyl esters form 2,4-dihydroxy-3-pyridinecarboxylic acid esters. Under the same conditions nitromalonic acid alkyl esters lead to 4,6-dihydroxy-3-pyridinecarboxylic acid esters, which also arise in the thermal cyclization of malonic acid 2,4,6-trichlorophenyl ester. The structure of the reaction products is determined by the relative nucleophilicity of the cyclization components.     

Liquid phase oxidation of 2-methyl pyridine to 2-pyridinecarboxylic acid over cobalt-doped SBA-3

Cobalt-doped SBA-3 was synthesized by cogellation method and was used as a catalyst for the oxidation of 2-methyl pyridine in acetic acid using aqueous hydrogen peroxide as oxidant. The catalyst exhibited very high substrate conversion (98%) and good product (2-pyridinecarboxylic acid) selectivity (93%). Fast hot catalyst filtration experiment proved that the catalyst acted as a heterogeneous one and it can be reused two times without losing its activity to a greater extent. The catalyst was characterized by X-ray diffraction, N₂ physisorption, diffuse reflectance UV–vis, and FT-IR.     

2甲-基吡啶在丙酮-水混合溶剂中的电氧化

在质子交换膜为隔膜的电解槽内,以2甲-基吡啶为原料,在丙酮/水混合溶剂中,以PbO2为阳极,电氧化合成了2-吡啶甲酸。通过循环伏安、线性扫描伏安和恒电位电解实验,考察了丙酮与水体积比、反应温度、硫酸浓度、反应物2-甲基吡啶浓度和阳极电位对选择性和电流效率的影响。结果表明,V(丙酮)∶V(水)=3∶1,硫酸浓度1.0~1.2 mol/L,2甲-基吡啶浓度0.5 mol/L,温度30℃,阳极电位1.75~1.80 V,生成2吡-啶甲酸的选择性可达88.7%,电流效率达到48.3%。而在纯水作溶剂的溶液中,相同条件下生成2-吡啶甲酸的选择性和电流效率仅分别为67.4%和42.2%。     

Synthesis and recognition properties for copper ions and cyanide anions of two coumarin hydrazide compounds

Two coumarin hydrazide compounds were synthesized by 7-N,N-diethylaminecoumarin-3-formyl chloride and 2-pyridinecarboxylic acid hydrazide or benzoylhydrazine. The compounds are found to be able to recognize copper ions and cyanide anions accompanied by obvious UV–vis absorption change and fluorescence turn-off response. Mechanism studies suggested that complexation between compounds and copper forms and cyanide may be bonded to 4-position of coumarin.     

Preparation of pyridinemonocarboxylic acids by catalytic vapour phase oxidation of alkylpyridines. I. Oxidation of 2- and 3-picoline and decarboxylation of 2- and 3-pyridinecarboxylic acid in the vapour phase

The vapour phase oxidation of 2-picoline with air using a singly promoted vanadium catalyst (V₂O₅/SnO₂, mole ratio 1/1.5), at a temperature of 375°C and a space velocity of 6130 h^?1, gave a 69% conversion with a selectivity of 64% for 2-pyridinealdehyde. No pyridoin formation was detected. In the vapour phase oxidation of 3-picoline using a doubly promoted vanadium catalyst (V₂O₅-TiO₂-Na₂O with V/Ti/Na=100/20/1.15) at a temperature of 400°C and a space velocity of 1450 h^?1, a 94% conversion of 3-picoline was obtained with a selectivity of 51% for niacin (3-pyridinecarboxylic acid) and 1% for 3-pyridinealdehyde. By varying the atom ratio V/Ti, the catalyst V/Ti = 100/25 was found to be the most active one. The decarboxylation of 2- and 3-pyridinecarboxylic acid in the vapour phase was also investigated under the conditions used in the oxidation of the picolines to the acids. At 350°C about 90% decarboxylation of picolinic acid occurs under these conditions, while only a few per cent of the niacin decarboxylated to pyridine between 300 and 500°C.     

Diastereoselective hydrogenation of 4-(phosphonomethyl)-2-pyridinecarboxylic acid

A Pd–Rh mixed metal catalytic system was developed that is able to hydrogenate 4-(phosphonomethyl)-2-pyridinecarboxylic acid to give 4-(phosphonomethyl)-2-piperidinecarboxylic acid with a cis selectivity of up to 98% with acceptable reaction time and without leading to metal contamination of the product. This revised version was published online in June 2006 with corrections to the Cover Date.     

金属卟啉仿生催化氧气氧化4-甲基吡啶制备异烟酸

研究了一种以金属卟啉为仿生催化剂,催化氧气液相氧化4-甲基吡啶绿色合成异烟酸(4-吡啶羧酸)的新方法。考察了不同金属卟啉对反应活性和目标产物选择性的影响,发现所有金属卟啉均具有良好的催化活性。系统地考察了温度、时间、氧气压力及催化剂浓度等因素对异烟酸选择性和收率的影响,结果表明,以5.0×10-5 mol/L的T(p-Cl)PPFeCl为催化剂,在1.25 mol/L的NaOH-EtOH溶液中于80℃、1.0 MPa的条件下反应8 h时,可得选择性为92.8%、收率为18.1%的异烟酸。