一种合成4-氰基联苯的方法

以联苯为原料,经傅克酰基化、氨解、脱水三步反应合成4-氰基联苯,不产生含氰废水。4-氰基联苯的总收率达到70.70%,HPLC含量达到98%以上。     

贵州水晶葡萄病原真菌分离鉴定及室内抑菌活性测试

[目的]确定引起贵州水晶葡萄采后贮藏病害的病原真菌种类及室内筛选用于该病害的主要防治杀菌剂。[方法]对病原菌进行分离纯化鉴定,通过科赫法则确定致病菌种类;筛选12种商品杀菌剂对炭疽病菌进行抑菌活性测定,筛选出有效药剂,为防治该病害提供一定的理论依据。[结果]从贵州省凯里市水晶葡萄采后贮藏病害分离鉴定出3株病原菌,为青霉菌(Penicillium sp.)、炭疽病菌(Clletotrichum gloeosporioides)和链格孢菌(Alternaria sp.),采用科赫法则,对3株病原真菌进行刺伤回接,发现3株均为水晶葡萄在贮藏过程中的主要致病菌。12种杀菌剂对水晶葡萄炭疽病菌进行室内抑菌活性测试结果表明:均具有较好的抑制活性,其中50%咯菌腈WP、50%苯菌灵WP、42%噻菌灵SC和43%戊唑醇SC对水晶葡萄炭疽病菌抑制活性最好,其EC50值分别为0.1024、0.1386、0.1624、0.1974 mg/L。[结论]凯里水晶葡萄采后病害病菌为青霉菌、炭疽病菌和链格孢菌;筛选出12种药剂针对水晶葡萄采后病害炭疽病菌的药剂,其中50%咯菌腈WP对炭疽病菌具有较好抑制效果,为水晶葡萄采后贮藏病害防治提供理论基础。     

Synthesis and structure of AlPO4-9: An unacquainted member in the family of microporous aluminophosphates

In the family of microporous aluminophosphate, AlPO₄-9 is one of the members reported first in 1982. However, its structure and characteristics have not been known up to now, and this makes it a special member. In the present work, AlPO₄-9 has been synthesized using piperazine as the structure-directing agent and the mixture of H₂O and EG as the solvent. Structure refinement from single crystal X-ray diffraction data shows that AlPO₄-9 is a material with the composition of C₂H₇Al_5.50NO₂₅P₆. It crystallizes in the monoclinic space group C2/c (No: 15), with a = 24.230(5) Å, b = 14.026(5) Å and c = 16.197(3) Å, β = 119.87(4)°, V = 4773(2) Å³, Z = 8. The open-framework of AlPO₄-9 is built of alternating corner-sharing PO₄ tetrahedra and AlO₄ tetrahedra (AlO₆ octahedra) to construct a curved one-dimensional 8-ring channel system running along [1 0 1]. Meanwhile, the strict alternative of PO₄ tetrahedra and AlO₄ tetrahedra (AlO₆ octahedra) results in a negative framework in AlPO₄-9. Thermal stability has been determined on a thermal analyzer and by calcination. It reveals that AlPO₄-9 framework is thermally stable and has a potential to be a catalytic material.     

High Resolution Crystal Structures of the Cerebratulus lacteus Mini-Hb in the Unligated and Carbomonoxy States

The nerve tissue mini-hemoglobin from Cerebratulus lacteus (CerHb) displays an essential globin fold hosting a protein matrix tunnel held to allow traffic of small ligands to and from the heme. CerHb heme pocket hosts the distal TyrB10/GlnE7 pair, normally linked to low rates of O(2) dissociation and ultra-high O(2) affinity. However, CerHb affinity for O(2) is similar to that of mammalian myoglobins, due to a dynamic equilibrium between high and low affinity states driven by the ability of ThrE11 to orient the TyrB10 OH group relative to the heme ligand. We present here the high resolution crystal structures of CerHb in the unligated and carbomonoxy states. Although CO binds to the heme with an orientation different from the O(2) ligand, the overall binding schemes for CO and O(2) are essentially the same, both ligands being stabilized through a network of hydrogen bonds based on TyrB10, GlnE7, and ThrE11. No dramatic protein structural changes are needed to support binding of the ligands, which can freely reach the heme distal site through the apolar tunnel. A lack of main conformational changes between the heme-unligated and -ligated states grants stability to the folded mini-Hb and is a prerequisite for fast ligand diffusion to/from the heme.     

半水磷酸晶体生产操作要点及存在问题的研究

瓮福集团公司为了降低液态磷酸在销售中物流成本高的问题,对w(H3PO4)85%的磷酸采用结晶工艺。介绍半水磷酸晶体生产工艺、操作要点,为解决生产中出现结晶槽盘管易结垢、产率低所采取的措施,以及研发磷酸深度冷却结晶工艺在实验室和工业上应用取得的效果。     

Increasing the X-ray Diffraction Power of Protein Crystals by Dehydration: The Case of Bovine Serum Albumin and a Survey of Literature Data

Serum albumin is one of the most widely studied proteins. It is the most abundant protein in plasma with a typical concentration of 5 g/100 mL and the principal transporter of fatty acids in plasma. While the crystal structures of human serum albumin (HSA) free and in complex with fatty acids, hemin, and local anesthetics have been characterized, no crystallographic models are available on bovine serum albumin (BSA), presumably because of the poor diffraction power of existing hexagonal BSA crystals. Here, the crystallization and diffraction data of a new BSA crystal form, obtained by the hanging drop method using MPEG 5K as precipitating agent, are presented. The crystals belong to space group C2, with unit-cell parameters a = 216.45 Å, b = 44.72 Å, c = 140.18 Å, β = 114.5°. Dehydration was found to increase the diffraction limit of BSA crystals from ~8 Å to 3.2 Å, probably by improving the packing of protein molecules in the crystal lattice. These results, together with a survey of more than 60 successful cases of protein crystal dehydration, confirm that it can be a useful procedure to be used in initial screening as a method of improving the diffraction limits of existing crystals.     

两种手性吲哚啉衍生物的合成与表征

以(S)-吲哚啉-2-羧酸为原料,经氮甲基化、酯化、格氏反应合成了两个未见文献报道的手性吲哚啉衍生物(S)-(1-甲基-2-吲哚啉基)二苯基甲醇和(S)-2-(1-甲基-2-吲哚啉基)-1,3-二苯基-2-丙醇,总收率分别达86.5%和89.7%,产物结构经1HNMR、13CNMR、HRMS确证。     

三维开放框架结构的无机-有机杂化材料[Cu4(SiW12O40)（pyz）4]的合成与晶体结构

以α-Keggin型硅钨酸、碳酸铜和2-乙基-3-甲基吡嗪(pyz)为原料,通过水热方法合成了标题化合物。采用元素分析、红外光谱和单晶X-射线衍射法表征了该化合物的结构。晶体结构分析表明,该化合物属于正交晶系,Pna21空间群,晶胞参数a=2.238 38(4)nm,b=1.386 87(3)nm,c=2.151 07(3)nm,α=β=γ=90°,V=6.677 7(2)nm3,Z=4,F(000)=6 408,Dc=3.598 g/cm3。该化合物中一价铜离子首先被pyz配体连接成波浪型的一维链状结构,而(SiW12O40)4-阴离子作为三齿配体进一步连接这些链形成一个三维的框架结构。     

肾上腺素的电化学氧化聚合研究

采用电化学石英晶振阻抗分析法,研究了金电极上肾上腺素(EP)循环伏安电氧化形成聚合膜的过程,并考察了溶液pH对聚合过程的影响。结果表明溶液pH在3.31和7.04间,肾上腺素的氧化产物发生环化反应后,进一步氧化在金电极表面沉积形成聚合膜,并提出了可能的聚合机理,且该聚合膜具有优良的阳离子选择渗透性。     

Upconversion Luminescence and Mechanism of Cerium Doped YVO4 Crystals

在 YVO4晶体中分别掺入摩尔分数为 2%的 Ce2（CO3）3和 CeO2,在中频感应加热炉中采用提拉法生长了掺 Ce 的 Ce：YVO4晶体。用 X 射线衍射测试了这两种晶体的物相,发现两种样品都主要以 YVO4相存在。X 射线光电子能谱测试表明,在两种样品中铈离子都是以＋3、＋4 混合价态的形式出现的。光谱测试表明,两种样品的光谱特性非常相似,同时发现,两种方式掺杂的 Ce：YVO4晶体在 620 nm 的光激发下,均可发出以 450 nm 为中心的蓝色宽带荧光。分析认为,在 Ce：YVO4晶体中由 620nm 引发的上转换发光的激发过程,不可能直接起源于 Ce3＋的基态2F5/2,它起源于由特殊的“Ce–O”构型形成的电荷迁移态的基态。