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In Chapter4, the reaction mechanism of phosphonyl nitrie oxides with acrylonitrile has been investigated.

为了简化计算模型,用甲基代替了膦酰基氧化腈中的异丙基进行模拟计算。

3 Recently, we reported an efficient tin-free version of this reaction involving thiophenol for the preparation of cyclopentane derivatives through a 1,5-hydrogen transfer/cyclization sequence [Eq.(1); AIBN=azobisisobutyronitrile].

最近,我们报道了高效的、不使用锡试剂而使用苯硫酚的反应,这个反应是通过1,5-氢转移/环化步骤制备环戊烷衍生物的[化学反应式(1);AIBN=偶氮二异丁腈][4]。

The conclusions were as follows: theνO-H andνC=O IR absorption maxima shifted towards higher wave numbers after imprinting 17β-estradiol on TFMAA-co-TRIM copolymer with the red shift of theνO-H groups being apparent after precipitation polymerization for 16h while that forνC=O groups being observed after polymerization for 24h. A strong interaction between TFMAA and 17β-estradiol was confirmed by the high selectivity for 17β-estradiol, as indicted by the values of the separation factor of isomers of 17β-estradiol/17α-estradiol (2.28) and the imprinted factor (3.01). Particle diameter of TFMAA-co-TRIM polymer was between 300 nm and 1.5μm, which suited well for solid phase sorbent throughout at low column pressure. The recognition of imprinting TFMAA-co-TRIM polymer for sterol molecules was driven by enthalpy eluted with acetronitile, and low temperature was in favor of the separation of sterol structure analogues on imprinting column. TFMAA-co-TRIM polymer possessed of determinate anti-heat stability, with melting point beginning at 255.84℃, Tp=257.40℃, control TFMAA-co-TRIM polymer and imprinting TFMAA-co-TRIM polymer were respectively decompounded at 267.79℃and 343.11℃, and solid micro-extraction noddle prepared by the special polymerization also showed definite recognition for 17β-estradiol by GC/MS detecting at 270℃. By selection of various washing and elution solvents, elution reagents of close polymerization system were of more advantage in template molecules retention and recognition on molecularly imprinted solid phase extraction column. At a certain extent, progesterone, 17α-estradiol, 17β-estradiol and 4-androstene-3, 17-dione could be intercepted on the MISPE column. Especially, MISPE had high selectivity for progesterone, and imprinting TFMAA-co-TRIM polymer could achieve adsorption balance within 50 min by absorption kinetics test for 17β-estradiol. However, MISPE column showed better selectivity and enrichment property for 17β-estradiol than C18 and CSPE columns according to the data from HPLC and GC/MS analyses. Recovery of 17β-estradiol on MISPE column was up to 85.5% while when prime extracting solution of milk powder was sampled, the recovery of CSPE and C18 columns were 43.7% and 30.7%, respectively.

通过研究阐明:紫外聚合产物TFMAA-co-TRIM中的νO-H振动吸收峰在聚合16h后红移,νC=O振动吸收峰在聚合24h后红移;TFMAA-co-TRIM对雌二醇异构体的印迹因子达到了3.01,α为2.28,优于其它功能单体参与得到的聚合物识别特性;TFMAA-co-TRIM聚合物粒径介于300 nm至1.5μm之间,作为色谱固定相具有良好的通量和低的柱压;在乙腈流动相中,TFMAA-co-TRIM分子印迹固定相的分离过程主要被焓驱动,低温有利于分子印迹固定相分离甾醇结构类似物;TFMAA-co-TRIM分子印迹聚合物在255.84℃时开始熔融,Tp=257.40℃,聚合物CP的降解温度在267.79℃,MIP降解温度在343.11℃,制备的固相微萃取头初步经GC/MS 270℃的耐热性测定;不同的洗提溶剂筛选证明了选择接近聚合溶剂的洗脱体系更有利于MISPE发挥识别效应;分子印迹固相萃取柱对孕酮、17α-雌二醇、17β-雌二醇和雄烯二酮都具有不同程度的保留特性,可作为此类化合物的吸附材料,特别对孕酮强保留的富集特性,可作为孕酮的选择性识别吸附剂,其分子印迹聚合物对17β-雌二醇的吸附动力学测定显示在50 min内基本达到吸附平衡,具有作为传感器核心敏感材料的潜力;对比萃取奶粉中17β-雌二醇性能,MISPE柱比非分子印迹固相萃取柱和C18柱具有更高的保留,回收率依次为85.5%,43.7%和30.7%。

For determination the content of isomaltooligosaccharide in beverage, a high performance liquid chromatography method was established by using 300 mm×4 6 mm, 5 μm Hypersil NH 2 column, acetonitrile+water=78+22 as mobile phase, detector was diffeential refractometer with 40℃ internal temprature.

为测定饮料中异麦芽低聚糖的含量,建立了使用 30 0mm× 4 6mm ,5 μmHypersil NH2 柱,乙腈+水=78+ 2 2为流动相,内部温度为 4 0℃的示差检测器的高效液相色谱法。

The catalytic system composed of NHPI and transition metal ion can catalyze effectively ethane into acetic acid,cyclane into dicarboxylic acid,toluene into benzoic acid,alkene into epoxide,alkyne into acetylenic ketone,and amide into imide;NHPI used alone can catalyze adamantane to be carbonylated,hydrogen peroxide prepared by oxidization alcohol;NHPI combined with as...

NHPI与过渡金属离子组成的催化体系能高效地催化乙烷氧化为乙酸、环烷烃氧化为二元羧酸、甲苯氧化为苯甲酸、烯烃氧化为环氧化物、炔烃氧化为炔酮、酰胺氧化为酰亚胺;NHPI单独使用能催化金刚烷发生氧化羰基化反应、催化氧化醇制取过氧化氢;NHPI与有机助催化剂如偶氮二异丁腈、溴化季铵盐、蒽醌和醇等也能催化分子氧氧化反应。

The same year with the Institute of Fine Chemicalto develop fine chemical products - o-aminobenzoic acid, and 1.4 million yuan of funds into an annual output of 200 tons built anthranilic acid production line, by the province for the Prohibition of Chemical Weapons Convention to fulfill the work of leadership Office approval in April 2002 with an annual output of 200 tons of the scale of operation, product quality compared with similar products in the domestic leading level, in October 2002 to carry out technical transformation again, the scale of production from 200 tons; years expanded to 500 tons; in size, and product performance, production capacity of plant expansion requirements, in 2003 officially put into operation. The end of 2004 our company moved to Sequoia small city are on the 1st, covering over 20,000 square meters, anthranilic acid after the removal of the production line expanded to 1200 tons; in size, at the same time developed a 2,2 - Dithio Benzophenone acid, benzo-iso thiazoline -3 - one, dichloro-acetonitrile, thiophene tons of ketones, a series of inter-amino benzoic acid, etc. Fine Chemical Products.

同年公司与上海桑迪精细化工研究所合作开发精细化工产品—邻氨基苯甲酸,并投入140万元资金建成了年产200吨邻氨基苯甲酸生产线,经省履行禁止化学武器公约工作领导小组办公室批准于2002年4月以年产200吨的规模投入运行,产品质量与国内同类产品相比处于领先水平,2002年10月公司再次进行技改,把生产规模由原来的200吨;年扩到500吨;年规模,且产品性能、生产装置能力达到扩产的要求,2003年正式投入运行。2004年末我公司搬迁至杉城小均1号,占地2万多平方米,搬迁后邻氨基苯甲酸生产线扩大到1200吨;年规模,同时开发了2,2-二硫代二苯甲酸、苯并异噻唑啉-3-酮、二氯乙腈、噻吨酮、间氨基苯甲酸等一系列化工精细产品。

The controlled/living radical polymerization of methacrylates containing carbazolyl or 1,3,4-oxadiazolyl groups via RAFT polymerization was successfully demonstrated. Functional polymers poly, poly, poly, and poly with hole- or electron-transfer ability were synthesized with cumyl dithiobenzoate as a chain transfer agent and AIBN as an initiator in a benzene solution.

以合成的二硫代苯甲酸酯异丙苯酯为链转移剂、偶氮二异丁腈为引发剂,通过RAFT可控/活性自由基聚合方法成功地合成了侧链上悬垂空穴传输基团或电子传输基团(1,3,4-噁二唑基团)的光电功能聚合物:poly、poly和poly、poly。

In this paper several methods including acylamide dehydration, metal cyanide replacement, etherification and isoxazole method for synthesis of 3,3-diethoxyethylcyanide were reviewed.

综述了3,3-二乙氧基丙腈的合成方法,包括酰胺脱水、金属氰化物取代、醚化和异恶唑法,用于工业化生产较为满意的合成路线是以1,1,3,3-四乙氧基丙烷为原料的异恶唑法。

This thesis is constituted by four parts: In the first part a summarization is given on the main total synthetic methods of isoflavones, for example, deoxybenzoin method which generally involves two steps wherein a phenol is reacted in the presence of a Lewis acid with phenylacetic acid to generate an intermediate deoxybenzoin which is then cyclized with a one carbon electrophile.

本论文主要工作包括四部分:第一章综述了近年来全合成异黄酮的主要方法:脱氧安息香法,是以多羟基苯酚与苯乙酸或苯乙腈在Lewis酸存在下,反应生成中间体脱氧安息香,然后再与亲电碳试剂进行关环反应生成异黄酮。

A micro-monolithic column was prepared by in-situ free radical polymerization of stearyl methacrylate with ethylene glycol dimethacrylate in the presence of the initiator AIBN and a mixture of porogens including iso-amyl alcohol and 1,4-butanediol.

以甲基丙烯酸碳酰十八酯为单体,乙叉二甲基丙烯酸酯为交联剂,异戊醇和1,4-丁二醇为二元致孔剂,偶氮二异丁腈为引发剂,原位制备了具有强疏水性的SMA整体微柱,并利用此整体微柱在普通高效液相色谱仪上测定滴眼液中氧氟沙星的含量。

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This one mode pays close attention to network credence foundation of the businessman very much.

这一模式非常关注商人的网络信用基础。

Cell morphology of bacterial ghost of Pasteurella multocida was observed by scanning electron microscopy and inactivation ratio was estimated by CFU analysi.

扫描电镜观察多杀性巴氏杆菌细菌幽灵和菌落形成单位评价遗传灭活率。

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