2-氧代-2-[(2-氯-5-吡啶甲氨基)(芳基)甲基]-4-芳基-5,5-二甲基-1,3,2-二氧膦杂环己烷的合成及其生物活性研究

通过类Mannich 反应“一锅法”合成了10个未见文献报道的含吡啶基的环状α-氨基膦酸酯, 其结构经¹H NMR, ³¹P NMR, IR, MS和元素分析确证. 测定了该系列化合物的杀虫、杀菌和除草活性, 结果表明, 所测化合物的杀虫活性不太好, 但所有化合物在药液浓度为1.0×10^－4 g/mL 时都具有较好的除草活性, 部分化合物在5.0×10^－5 g/mL时显示出良好的杀菌活性.     

二次乳化法(W/O)/W制备蛋白质流通色谱固定相的研究

以甲基丙烯酸缩水甘油酯为单体,二甲基丙烯酸乙二醇酯为交联剂,甲苯与正庚烷为有机致孔剂,20%的甘油水溶液为内水相(超孔致孔剂),利用二次乳化法制备了(W/O)/W乳液,通过紫外光引发悬浮聚合生成两类孔型高分子微球(BiPB).BiPB孔径为双峰分布,范围分别在10~100nm和1000~7300nm之间;而其体积平均粒径、比表面积、湿密度、静态吸附容量与不含超孔的微孔介质(MiPB)接近.修饰相同二乙胺密度的BiPB和MiPB介质虽在较低流速(5cm/min)下有相近的动态吸附容量,但在高流速(40cm/min)下BiPB的动态吸附容量约为MiPB的动态吸附容量的3倍,表明BiPB介质的超孔结构对孔内传质的强化作用,因而其更适合于高速的蛋白质色谱分离.     

一步法合成吲哚用Ag／SiO2催化剂的失活及其抑制

 用简单浸渍法制备了Ag／SiO2催化剂．该催化剂对苯胺和乙二醇一步合成吲哚表现出很高的催化活性，但同时存在明显的失活．TG，XRD和TEM表征结果表明，催化剂失活的主要原因是反应过程中催化剂表面的积碳和银粒子的烧结．向反应体系中通入氢和水蒸气能够减少催化 剂表面的积碳；向催化剂体系加入ZnO助剂能较大程度地提高银的分散度，并能有效抑制反应过程中银粒子的烧结．     

聚酰亚胺中空纤维膜用于甲醇/甲基叔丁基醚的分离

甲醇／甲基叔丁基醚混合物的膜法分离，大多采用渗透汽化方法，少有采用蒸汽渗透法。用聚酰亚胺中空纤维膜，对以蒸汽渗透和渗透汽化两种方式分离甲醇／甲基叔丁基醚混合物（甲醇质量分数为0．01－0．30）的效果进行了对比。结果显示，在甲醇质量分数低于0．05时，蒸汽渗透较渗透汽化法的分离性能优越。     

A Novel, Simple and Efficient Synthesis of Ferrocenyl Enones and Alkynols

Propargylic alcohols are versatile precursors to many organic molecules including natural products and pharmaceutical compounds.[1] In our continuing interest in the development of practical methods for synthesis of ferrocene derivatives, we decided to investigate the efficiencies of ferrocenylacetylene addition to aromatic aldehydes under t-BuOKcatalyzed condition.[2] Interestingly, we found that the usually reliable coupling reaction between terminal alkyne of type 1 and aromatic aldehydes of type 2 does not furnish the expected propargylic alcohols, but that the isomeric aryl enones 3are found in high yield and very short reaction time (10～20 min). This provided a promising protocol for preparation of ferrocenyl chalcones in a practical, economical and mild sense compared with the traditional method. To the best of our knowledge, this unusual reaction was first observed for the addition of ferrocenylacetylene to aldehyde in a base-catalyzed manner (Eq. 1).     

Baylis-Hillman Reactions of Sulfonyl Aldimines or Aryl Aldehydes with 3-Methylpenta-3,4-dien-2-one or 3-Benzylpenta-3,4-dien-2-one

The attempted Baylis-Hillman reactions of sulfonyl aldimines or aryl aldehydes with 3-methylpenta-3,4-dien-2-one or 3-benzylpenta-3,4-dien-2-one gave the corresponding Baylis-Hillman adducts in moderate yields in DMSO under the catalysis of DBU or PMe3, respectively. Moderate diastereoselectivities were observed in the reaction of 3-benzylpenta-3,4-dien-2-one with N-arylmethylidene-1-naphthalenesulfonamides catalyzed by chiral catalyst cinchona alkaloid derivative TQO {4-（3-ethyl-4-oxa-1-azatricyclo[4.4.0.0^3,8]dec-5-yl）quinolin-6-ol}.     

Microwave-Assisted Olefination Reaction of Alkylzinc with Aromatic Aldehyde Catalyzed by Nickel Complex

Carbon-carbon double bond-forming reactions have always been great importance in organic synthesis. Manymethods have been described for C =C bond formation. We[1] have reported the new method of C =C bond formation of nickel catalyzed organozinc with aromatic aldehydes in the presence of Me3SiC1.     

Crystal Structure of (1R,4R;1S,4S)2-Amino-3-Cyano-1,4-Diphenyl-2-Cyclopentene-1-ol

1INTRODUCTIONIntheearly1970'sthreegroupsofinvestigatorsL,~,'foundthatlow-valenttita-nium,preparedbythereactionofstrongreducingagentswithtitaniumtrichlorideortitaniumtetrachlorideintetrahydrofuran,canabstractoxygenfromketonesoraldehydes,leadingtotheforma-tionofolefins.Theinterestinthereactioninducedbylow--valenttitaniumreagentsisincreasingandalargenumberoffunctionalgroupscanbereduceds4-6).Recent-ly,wefoundthatthetitlecompoundisObtainedbycy-cllzatlonreactionof(3--oxo-1,3-diphenyl)propyl-pro…     

低价钛引起的芳酮肟的反应

在低价钛试剂 (TiCl4/Sm)作用下取代苯乙酮肟发生脱肟反应生成酮 ,而在同样条件下 ,二芳酮肟则生成二芳酮、胺或希夫碱     

TiO2-双亲共聚物复合纳米粒子的合成与紫外光敏特性

用偶联剂乙烯基三乙氧基硅烷改性纳米粒子TiO₂, 应用超声技术将TiO₂ 纳米粒子分散在甲醇介质中, 然后用苯乙烯(ST)原位聚合包封, 再用丙烯酰胺或乙烯基吡咯烷酮(VP)共聚, 两步原位分散聚合得到了有机聚合物为壳、TiO₂为核的有机/无机复合粒子. 用红外光谱、紫外-可见光谱、透射电子显微镜等检测手段进行表征. 结果显示: 由于双亲共聚物对TiO₂纳米粒子的敏化作用, 紫外-可见光谱图上两种纳米复合粒子的最大吸收峰均有明显红移, 并且吸收光谱的范围扩大了, 其中尤以TiO₂/(PST-co-PVP)为甚. 意味着光敏化活性的提高, 特别是在可见光谱的范围内. 这种情形对宽带隙半导体材料如TiO₂纳米粒子的光催化特性是有利的, 表明这类材料的应用空间得到了拓展.