Synthesis of tetrahydrofolate coenzyme models 1,2-dimethyl-3-m(p)-nitrophenylsulfonyl imidazolinium iodide and their methyl-substituted one carbon unit transfer reactions

Tetrahydrofolate (THF) coenzymes are involved in biochemical transfer of aone-carbon fragment at different oxidation levels. The study of THF models may providea valuable class of reagents for group transfer reactions with practical significance. Onlya few researches about 5, 10-methenyl-THF models have been reported in literature.

Synthesis and Crystal Structure of Trans-4-[(5-(2,4-Dichlorophenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one

The title compound trans-4-[（5-（2,4-dichlorophenoxy）-3-methyl- 1-phenyl-1H-pyrazol-4-yl）methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 （C28H23Cl2N5O2, Mr = 532.41） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438（4）, b = 11.6065（5）, c = 14.2215（6）A, α = 112.566（1）, β = 92.324（2）, γ = 102.91（1）°, V= 1315.65（10） A^3, Z = 2, Dc = 1.344 g/cm^3,μ（MoKa） = 0.282 mm^-1, λ = 0.71073 A, F（000） = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C（ 12）-H（12）…O（1） and C（28）-H（28）...O（1）# 1 hydrogen bonds were observed in the title compound.

Synthesis, Crystal Structure and Antitumor Activity of (E)-1-(7-Methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5- yl)-3-(2-methoxyphenyl)-2-(1H-1,2,4-triazol-1-yl)propenol

The title compound, （E）-1-（7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl）- 3-（2-methoxyphenyl）-2-（1H-1,2,4-triazol-1-yl）propenol （3a）, was synthesized by the Aldol con- densation reaction of 1-（7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl）-2-（1,2,4-triazol- 1-yl）ethanone with 2-methoxybenzaldehyde and then reduced with NaBH4, and its crystal structure was determined by single-crystal X-ray diffraction： monoclinic system, space group P21 with a = 6.2002（3）, b = 12.8452（7）, c = 13.2257（7） ？, Z = 2, V = 1031.23（9） ？3, Mr = 407.46, Dc = 1.312 Mg/m3, S = 1.054, μ = 0.091 mm-1, F（000） = 432, the final R = 0.0353 and wR = 0.0769 for 3161 observed reflections （I 〉 2σ（I））. X-ray analysis displays that the title compound adopts an E configuration for the C（7）=C（8） double bond and S configuration for the chirality center with the specific rotation of –63.75°. Furthermore, the stability of the crystal was maintained through the intermolecular hydrogen bond O（1）–H？？？N（3）. The antitumor assay exhibits that the title compound 3a （E configuration） has a good antitumor activity against the Hela cell line with the IC50 value of 36.9 μM, which is better than that of 3b （Z configuration）.

固体强酸催化剂S_2O_8^(2-)/ZrO_2-Al_2O_3-M_2O_3(M=Cr,Ce,La)的制备

Three kinds of new type solid strong acid catalysts S2O 2-8/ZrO2-Al2O3-M2O3（M=Cr,Ce,La） were prepared. Their crystal structure, surface area, acid strength and sulfur content were determined by means of XRD, BET, flow Hammett indicator method and chemical analysis. Their catalytic activities in esterification reaction of acetic acid with n-butanol were studied. The results showed that ZrO2 in the catalysts mainly in tetragonal phase and few in monoclinic phase. The tetragonal phase of ZrO2 and S2O 2-8 are the key factors that guarantee the catalytic activity. Incorporation of appropriate amounts of metallic oxides（Cr2O3,Ce2O3,La2O3） into the catalyst favors the stabilization of sulfur species and surface area, which increase the activity sites on the catalyst. The experimental results showed that three catalysts S2O 2-8/ZrO2-Al2O3（2%）-M2O3（1%）（M=Cr,Ce,La） had higher catalytic activity in mentioned esterification, with the conversion of acetic acid reached 96.8%, 95.7% and 96.1%, respectively. The preparation condition of the catalysts showed great influence on the catalytic activity.

超音速火焰喷涂WC-Cr_3C_2-M涂层性能及其在液压支架立柱上的应用研究

分别采用电镀和超音速火焰喷涂在27SiMn钢表面制备了硬铬和WC-Cr_3C_2-M涂层,测试了两种涂层的机械性能以及磨损和腐蚀性能,并将WC-Cr_3C_2-M涂层在煤矿的液压支架的立柱上井下应用。结果表明:相对于电镀硬铬涂层,采用超音速火焰喷涂工艺制备的WC-Cr_3C_2-M涂层与基体结合强度高,孔隙率低,表现出更高的硬度、耐磨和抗腐蚀性能。WC-Cr_3C_2-M涂层在井下实际工况下防护效果显著,可以代替会给环境带来严重污染的电镀硬铬,用于煤矿井下的液压支架的表面防护。

Synthesis, Crystal Structure and Fungicidal Activity of (Z)-3,3-Dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one O-2-Chlorobenzyl Oxime Nitrate

The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481（8）, b = 9.3351（5）, c = 13.1911（7） , β = 98.9450（10）°, Z = 4, V = 1769.67（17） 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F（000） = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections （I 2σ（I））. X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.

Synthesis, Crystal Structure and Property of a Series of Supramolecular Polymers Based on Novel 3,5-Dimethyl- 2,6-bis(3-(pyrid-2-yl)-1,2,4-triazolyl)pyridine Ligand

Solvothermal reactions of 3,5-dimethyl-2,6-bis（3-（pyrid-2-yl）-1,2,4-triazolyl） pyridine （L）, 1,4-benzendicarboxylic acid （H2bdc）, and transitional metal cations of M11 （M = Mn, Co, Cd） in the presence of oxalic acid （H2ox） afford three novel supramolecular polymers （CPs）, namely, {[M2（ox）（L）2][bdc][M2（Hox）2（OH）（H2O）4]·3H2O}n （M = Mn for 1, Co for 2, Cd for 3）. Single-crystal X-ray diffraction analysis reveals that complexes 1-3 are isostructural and the 3D supramolecular structure was connected through non-covalent interactions. With the help of H2ox, the L ligands cheated with center atoms forming a butterfly [M2（ox）（L）2]2＋ building block. The bdc2- ligand linked with the unprecedented [M2（Hox）2（OH）2（H2O）4] units through strong O-H...O hydrogen bonds forming a zigzag chain, which are further connected through π-π interactions between L and bdc2- ligands to form a 3D supramolecular structure. Moreover, elemental analyses, IR, thermogravimetric, PXRD and luminescence have been investigated.

An efficient synthesis of 2,2′-arylmethylene bis-(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) and 1,8-dioxooctahydroxanthenes using ZnO and ZnO-acetyl chloride

2,2'-Arylmethylene bis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) 4l-s produced from reaction between dimedone with various aldehydes in acetonitrile using ZnO as a catalyst;whereas in the presence of ZnO-acetyl chloride catalysts the reaction is limited to give only 1,8-dioxo-octahydroxanthenes 3a-k in very good yields.

甲亢患者尿Alb、IgG和β_2-m联检与FT_3、FT_4、TSH诊断的相关性分析

甲状腺功能亢进症（简称甲亢）是影响终身健康的常见病、多发病，是指由各种病因导致的甲状腺功能增强，甲状腺激素（thyroid hormone，TH）分泌过多而引起的甲状腺毒症。而甲亢的早期具有明显的肾脏功能的改变，

Synthesis and Bioactivity of Novel Aminomethyl-2-(1,2,4-triazol)-4,4-dimethyl-3-pentanone(ol)

Dimethyl-1-(1, 2, 4-triazol) -2- butanone was treated with aqueous formaldehyde to give an additional product, and subsequent elimination by acetic anhydride yielded 4, 4-dimethyl-2-(1, 2, 4-triazol)-1-penten-3-one. Further addition with substituted amines provided a series of (1, 2, 4-triazol)-4, 4-dimethyl-3-pentanone, which were then reduced by KBH4 to obtain a series of (1, 2, 4-triazol)-4, 4-dimethyl-3-pentanol. Their structures were confirmed by 1HNMR and elemental analysis. The results of bioassay showed that the title products possess good fungicidal activities.

Synthesis of (R)(E)-3,7-Dimethyl-2-octene-1,8-dioic Acid, a Copulation Released Pheromone Component of Azuki Bean Weevil

Started from 5-hydroxy-2-pentanone, (R)(E)-3,7-dimethyl-2-octene-1,8-dioic acid, callosobruchusic acid, was synthesized via five steps with D-(-)-camphor sultam as the chiral auxiliary. It was of good optical purity and yield.

4-[(Furan-2-ylmethylene)-amino]-1,5-dimethyl-1,2-dihyl-1,2-dihydo-pyrazol-3-one

The title compound （C16H15N3O2, Mr= 281.31） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the C=N double bond. It crystallizes in the monoclinic system, space group P2 1/c with a = 11.150（3）, b = 9.906（3）, c = 13.624（4） A, β = 106.360（4）°, V= 1443.9（7） ,A^3, Z = 4, Dc = 1.294 g/cm^3, F（000） = 592,μ（MoKa） = 0.088 mm ^-1, R = 0.0577 and wR = 0.1214. Of the 5766 total reflections, 2540 were unique. In the molecule there exist two different planes of pyrazoline and O（2）-C（10） phenyl ring, which are approximately coplanar （r.m.s. de deviation from the combined mean plane is 0026 A） with the dihedral angle between them of 6.3°.

40例糖尿病患者T_3、T_4、TSH、β_2-m球蛋白测定及分析

1999年1～9月,笔者将糖尿病患者的血清作了T3、T4、TSH、β2-m球蛋白的测定,对其临床意义进行了探讨.现报告如下.

50例糖尿病患者T_3、T_4、Tsh、β_(2-m)球蛋白测定及分析

2001-02～2001-11我们将糖尿病患者的血清作了T3、T4、Tsh、β2-m球蛋白的测定,对其临床意义进行了探讨,报告如下.

实用优先 精英B75H2-M3主板

精英B75H2-M3虽然采用的Micro ATX板型,但整体布局走线仍井然有序。产品配备4+1+1相供电设计,有效满足全系列LGA1155接口处理器的需求。产品的内存插槽虽然缩减为两条,但仍然能支持双通道DDR31600内存。

基于STM32F10X引导程序实现USB在应用中编程

基于芯片固化的Bootloader基础上,研究USB在IAP编程中应用的方法,分析Cortex2-M3核的存储器组织结构及启动模式、配置和访问机制,IAP实现的机理,给出了通过USB接口实现IAP的步骤和编程要点,下载的保障机理,并对IAP下载的应用程序编写和实现进行说明。相对串口下载,系统数据下载速度极大改善,提高下载效率。

Enzymatic Synthesis and Characterization of Novel Polycarbonates Derived from 5-Allyloxy-1, 3-dioxan-2-one and 5, 5-Dimethvl-1.3-dioxan-2-one

Novel polycarbonates from 5-allyloxy-1, 3-dioxan-2-one （ATMC） with 5, 5-dimethyl- 1, 3-dioxan-2-one （DTC） were successfully synthesized for the first time using immobilized porcine pancreas lipase （IPPL） as catalyst. The resulting copolymers were characterized by IR, ^1H NMR, ^13C NMR and GPC. The molecular weight （Mn） of the copolymer with molar feed ratio of 10：90 （ATMC：DTC） was 9300 and the polydispersity was 1.31, while the Mn increased to 14300 and polydispersity of 1.25 with the feed ratio of 50：50. Moreover, the composition of the copolymers agreed well with the monomer feed.

草苁蓉中2个单萜苷类化合物的NMR研究

从草苁蓉75%乙醇提取物中分离得到了2个单萜苷类化合物,结合其理化性质,并通过1DNMR(1 H NMR,13 C NMR)及1 H-1 H COSY、HSQC、HMBC、NOESY等多种波谱学方法进行结构鉴定,鉴定2个化合物分别为β-D-glucopyranose 1-(3,7-dimethyl-2-trans-6-octa-dienoate)(化合物1)和6,7-dihydrofoliamenthoic acid diglucoside(化合物2),其中化合物1为新化合物,化合物2为第1次从列当科植物中获得.