从磷硅试剂合成烃基膦酯类化合物

本文报导三甲基硅氧基亚磷酸酯(一种活性较高的磷硅试剂)与醛酮反应而获得十四个二乙基三甲硅氧基烃基膦酸酯。产物结构经IR,~1HNMR,~(31)PNMR,MS测试和元素分析表征;对反应机理作了初步讨论。     

主链含膦酸酯的聚酸酐药物控制释放材料研究

通过二氯膦甲（乙）酸乙酯与对羟乙氧基苯甲酸反应，制备了二羧苯氧乙氧基膦甲（乙）酸乙酯，并其转化成混合醋酐并通过熔融缩聚，合成了主链含膦甲（乙）酸乙酯的聚酸酐，以二羧苯氧乙氧基膦甲（乙）酸乙酯，分别与１，３－双（４－羧基苯氧基）丙烷（ＣＰＰ）及癸二酸（ＳＡ）共聚，得到相应的共聚酸酐，对所合成的单体和聚合物的结构进行了表征，研究了它们的体外降解，酶促降解及其对抗肿瘤药物５－氟尿嘧啶和氨甲喋蛉的释放性能     

4’，5，7－三羟基－2’－甲氧基－6，8－二异戊烯基黄烷酮的全合成

以２，４，６－三羟基苯乙酮和间甲氧基苯酚为原料，分别经过异戊烯基化和保护羟基以及甲醛化，保护羟基，再通过缩合、环化、去甲氧基甲基等共七步反应，首次成功地合成了４’，５，７－三羟基－６，８－二异戊烯基黄烷酮。     

合成2—芳氧基—5—氟—3H—4—嘧啶酮的新方法

由２－氰－５－氟－３Ｈ－４－嘧啶酮和取代苯酚钠在常压下反应，合成了７个未见文献报道的２－芳氧基－５－氟－３Ｈ－４－嘧啶酮化合物，产率７０￣８７％，结构经ＩＲ、＾１Ｈ ＮＭＲ和ＭＳ证实。     

2—Hydroxynepthenol的关键前体—3,7,11,15—四甲基—14—氧化—15—叔丁基 …

以香叶基丙酮为起始原料，经五步反应以３２％的总收率首次合成了３，７，１１，１５－四甲基－１４－氧代－１５－叔丁基二甲基硅氧基－２Ｅ，６Ｅ，１０Ｅ－十六碳三烯酸乙酯，它是２－Ｈｙｄｒｏｘｙｅｎｅｈｐｔｈｅｎｏｌ全合成中的酮酯关环前体。     

The First Synthesis of Ethyl 3,7,11,15-Tetramethyl-14-oxo-15-tert-butyldimethylsiloxy-2E,6E,10E-hexadecatrienoate——The Key Precursor of 2-Hydroxynephthenol

以香叶基丙酮为起始原料，经五步反应以３２％的总收率首次合成了３，７，１１，１５－四甲基－１４－氧代－１５－叔丁基二甲基硅氧基－２Ｅ，６Ｅ，１０Ｅ－十六碳三烯酸乙酯。它是２－Ｈｙｄｒｏｘｙｎｅｐｈｔｈｅｎｏｌ全合成中的酮酯关环前体。     

用色谱—质谱和质量以谱研究苯甲酸钐热分解反应

为合成某些芳香族有机化合物提供一种新途径，用色谱－质谱联用技术和质量色谱法研究了苯甲酸钐的热分解反应产物。其热分解产物溶入丙酮后有大量９，１０－蒽醌析出，其丙酮溶液中还含有１，２－二苯甲酰基苯（２５．６％）、苯甲酸（１８．７％）、二苯酮（１４．４％）、９－勿酮（８．２％）、９－苯甲勿（４．９％）、取苯（３．６％）、二苯甲烷（２．３％）、３－甲酰苯基联苯（２．１％）、二苯基乙二酮（１．９％）、４－甲     

2,3－二甲基－4－甲氧甲酰－2－环己烯醇的合成

2;3－二甲基－4－甲氧甲酰－2－环己烯醇的合成;二甲基甲氧甲酰环己烯醇;甲基甲氧甲酰环己烯酮;二甲基甲氧甲酰环己烯酮;氢化钠;氢化三叔丁氧基铝锂     

1,3,4,6—四硫代戊搭烯—2,5—二酮制备含硫取代基的四硫富瓦…

以１，３，４，６－四硫代戊搭烯－２，５－二酮为原料，经偶联，醇解，烃化或醇解，烃化，偶联等步骤，制得四甲硫基四硫富瓦烯，四乙硫基四硫富瓦烃，二喹喔啉硫醚，４－甲硫基－５－甲氧甲酰硫基－１，３－二硫环戊烯－２－酮。四甲基乙烯和４，４＇－二甲硫基－５，５＇－二甲氧甲酰硫基四硫富瓦烯及它的异构体混合物，提出了１，３，４，６－四硫代戊搭烯－２，５－二酮醇解机理。讨论了未得到某些预期产物的原因，报道了３种四     

含1-(2-甲氧乙基)茚基和二(三甲硅基)胺基的稀土有机配合物的合成和表征

无水三氯化稀土（ＬｎＣｌ３），二（三甲硅基）胺基钾（ＬｉＮ（ＳｉＭｅ３）２〗及１－（２－甲乙基）茚室温上在四氢呋喃溶剂中反应，得到了４个含１－（２－甲氧乙基）茚基和二（三甲硅基）胺基的稀土金属有机物｛（Ｃ９Ｈ６ＣＨ２Ｃ２ＯＭｅ）Ｌｎ〖Ｎ（ＳｉＭｅ３）２〗２（Ｌｎ＝Ｎｄ，Ｓｍ，Ｄｙ，Ｙｂ）｝，这些配合物均经元素分析、ＩＲ和ＭＳ表征。     

Studies on silicon-containing fragrance raw materials I. Syntheses and structure-odor relationship of acetals of 4-trimethylsilyl-3-cyclohexenone and 4-trimethylsilylcyclohexanone and their carbon counterparts

In order to investigate the structure-odor relationship of odoriferous compounds and search for new aroma chemicals, seven acetals of 4-trimethylsilyl-3-cyclohexenone and their carbon counterparts were synthesized by Birch reduction of 4-substituted anisoles and then acetalization. Seven acetals of 4-trimethylsilylcyclohexanone and their carbon counterparts were synthesized similarly. Structures of all new compounds were determined by MS, IR and ¹H NMR , and their characteristic odors were evaluated as well. The characteristic odors of the acetals formed by 4-substituted-3-cyclohexenone and 1,2-diols are fruity and woody. The acetals formed from 1, 3-diols are woody, and formed with 1, 4-diols are very faint in odor. Odors of acetals of 4-substituted cyclohexanone are all very weak. As a whole, odors of organosilicon compounds are weaker, but somewhat more delicate than their carbon counterparts.     

ZnCo2O4纳米粒子的可见光催化性能

研究了共沉淀分解法制备的ZnCo₂O₄纳米粒子的光学和可见光催化性能,并对其晶体结构和微观结构用X射线衍射、热重/差热分析、透射电镜和高分辨透射电镜等手段进行了表征.结果表明,制备的纳米粒子为纯相的ZnCO₂O₄,平均粒径约为10-20 nm.紫外-可见吸收光谱估计出ZnCo₂O₄纳米粒子的能带隙为3.39和2.09 eV.可见光（λ>420 nm）照射下,纳米粒子表现出降解亚甲基蓝溶液的光催化活性.ZnCo₂O₄纳米粒子的光催化活性可以归结为紫外和可见光下纳米粒子吸收光子（能量大于能带隙）的能力,以及它们的纳米尺寸,基于实验结果,本文提出了ZnCO₂O₄可能的能带结构.     

Synthesis of 2-methyl-3-(3,5-diallyl-4-hydroxyphenyl)-4-quinazolones as possible anticonvulsants

A series of 2-methyl-3-(3,5-diallyl-4-hydroxyphenyl)-4-quinazolones were prepared as possible anticonvulsants. All compounds were evaluated for their anticonvulsant activity against pentylene-tetrazol-induced seizures and their ability to potentiate sodium pentobarbital sleeping time in albino mice.     

显影抑制剂释放化合物的合成

为寻找新的适用于不同情况的最佳品种显影抑制剂释放化合物(DIR化合物).合成了母体结构为1-苯基-2-乙酰氧基-2-[(1-苯基-1H-四氮唑-5-)疏基]乙酮的DIR化合物.在这一化合物的二个苯环中分别引入不同取代基制备了十四个新化合物.所有化合物以苯乙酮为骨架,1-(4'-取代苯)-5-疏基四唑部份为显影抑制剂.     

吡啶-2,6-二甲酸衍生物及其Tb(Ⅲ)和Eu(Ⅲ)配合物的合成与荧光性质

以吡啶-2,6-二甲酸(DPA)为起始物,合成了4-羟甲基吡啶-2,6-二甲酸(4-HMDPA)和4-(N,N-二羧甲基氨基)亚甲基吡啶-2,6-二甲酸(4-BMDPA)两种新型多功能配体,并制备了DPA,4-HMDPA及4-BMDPA的Tb(Ⅲ)和Eu(Ⅲ)配合物,对配合物的固体和溶液态的荧光性质进行了研究. 结果表明,在吡啶4位引入弱吸电子基团4-羟甲基会减弱稀土配合物的荧光强度; 在水溶液中稀土配合物与溶液的pH值有着密切的关联,中性水溶液中荧光强度较大; 分子偶极矩较小的溶剂中稀土配合物荧光强度较强. 表明4-BMDPA是较理想的稀土荧光敏化剂.     

New virescenosides from the marine-derived fungus Acremonium striatisporum

Five new diterpene glycosides, virescenosides Z4-Z8 (1-5) have been isolated from a marine strain of Acremonium striatisporum KMM 4401 associated with the holothurian Eupentacta fraudatrix. Their structures were determined by HRESI-MS and 1D and 2D NMR. Virescenosides Z4-Z8 contain rare altruronic acid 4C1 and 1C4 conformations as their carbohydrate components. Virescenosides Z5 and Z7 exhibit an unusual 16-chloro, 15-hydroxyethylgroup as their side chains.     

Research on aminomethylene derivatives of azoles

It is shown that, in contrast to hippuric acid, thiohippuric acid reacts with dimethylformamide in the presence of phosphorus oxychloride to give three compounds, viz., 2-phenyl-4-dimethylaminomethylene-5-thiazolone, 2-phenyl-4-dimethylamino-methyleneoxazole-5-thione, and 2-phenyl-4-formyl-5-chlorothiazole. The pathways of their formation are discussed. The structures of the compounds obtained and some transformations of 2-phenyl-4-formyl-5-chlorothiazole were studied. 2-Phenyl-4-formyl-5-hydroxy(mercapto) thiazoles and their methyl derivatives, as well as 2-phenyl-4-dimethylaminomethylenethiazole-5-thione, were synthesized from the latter.See [1] for Communication 23.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 36–39, January, 1980.     

Synthesis and structure of new 3,7-diazabicyclo[3.3.1]nonane derivatives

Aminomethylation of triethylammonium 4-aryl-3,5-dicyano-6-oxo-1,4,5,6-tetrahydropyridin-2-olates and their sulfur and selenium analogs, as well as the structure of formed products, were studied in details. The reaction is of general character and leads to the formation of 7-substituted 9-aryl-2,4-dioxo-, 9-aryl-4-oxo-2-thioxo-, 9-aryl-4-oxo-2-selenoxo-3,7-diazabicyclo[3.3.1]nonane derivatives or their salts. The structures of ethyl 9-(2-chlorophenyl)-5-cyano-7-(4-methylphenyl)-2-oxo-4-thioxo-3,7-diazabicyclo[3.3.1]nonane-1-carboxylate (as a complex with N-methylmorpholine) and triethylammonium salt of 7-benzyl-4-oxo-2-selenoxo-9-(2-thienyl)-3,7-diazabicyclo[3.3.1]nonane-1,5-dicarbonitrile were studied by X-ray crystallography.     

Interconvertible Eudesmanolides Containing a 6,12‐Hemiketal Function from Salvia castanea Diels f. tomentosa Stib.

Two new eudesmanolide sesquiterpenoids containing a hemiacetal function, castanins G and H ( 1 and 2 ), were obtained as a pair of interconvertible isomers from the aerial parts of Salvia castanea Diels f. tomentosa Stib. , and separated as their uninterconvertible acetates 3 and 4 . Their structures were elucidated by unequivocal interpretation and comparative analysis of the NMR and MS data of the mixture 1 / 2 and of their acetates 3 and 4 , respectively. The inhibitory activity of 3 and 4 toward MCF‐7, HeLa, and HepG2 cell lines was also evaluated.     

桑黄黄酮A和B的分离与合成

利用正相硅胶柱色谱，Sephadex LH-20柱色谱以及反相HPLC等手段从真菌桑黄 中分离得到两个新的二氢黄酮衍生物，经1D NMR，2D NMR和MS等光谱方法鉴定其结 构分别为5，7，4'－三羟基－6－邻羟苄基二氢黄酮和5，7，4'-三羟基－8－邻羟 苄基二氢黄酮，并且对它们进行了合成。