β—受体阻滞剂及其类似物的毛细管电泳手性分离

在毛细管电泳上对12种β－受体阻滞剂和类似物的光学对映体进行了分离,研究了它们的拆分条件。使用0.1mol/L,pH3.0的磷酸－三乙醇胺缓冲液,20kV电压,12－36mmol/L羟丙基－β－环糊精作为手性识别试剂。其中11种β－受体阻滞剂及其类似物以苯乙醇胺、胺酵素在50cm普通毛细管上获得了较好的手性分离效果,普罗勒沙的对映体在本条件下未获分离。同时发现,芳香环上取代基位置对迁移时间的影响有一定规律。     

N^2（p—甲基苯磺酰）—L—谷氨酰胺的晶体结构测定

谷氨酰胺衍生物抗瘤酮A_(10)(3-苯乙酰胺基-2,6-哌啶二酮)是从人尿、血液中分离出来的天然广谱性抗肿瘤活性化合物,无明显毒副作用,目前正进行Ⅱ期临床研究.其抗肿瘤的有效成分被认为是它的2个水解产物苯乙酰谷氨酰胶和苯乙酰异谷氨酰胺。De和Pal曾对抗瘤酮A_(10)的类似物如3-对甲苯磺酰胺基-2,6-哌啶二酮等做过抗艾氏腹水癌活性评价,探讨了构效关系.但未见这些化合物的空间结构和电子结构方面的报道.我们合成了抗艾氏腹水癌活性较高的化合物3-对甲苯磷酰胺基-2,6-哌啶二酮的水解产物——对甲苯磺酰谷氨酰胺,并测定了其晶体结构。为进一步研究其分子结构与抗肿瘤活性的关系提供结构数据。     

N—芳基—N‘—取代噻唑基脲的合成与结构表征

由于植物细胞分裂素在植物生长发育中非常重要的作用 ,一直得到人们的重视 ,但其天然存在量微难以大量应用 ,故人工合成的化学结构类似物相继出现 ,主要有嘌呤类 ,如 6-苄氨基嘌呤 ( 6-BA)等 [1]和脲类化合物 ,如二苯脲类 ( DPU) [2 ]和N-苯基 -N′-( 1 ,2 ,3 -噻二唑 -5 -基 )脲 ( TDZ) [3]。人工合成嘌呤类植物细胞分裂素的结构改造一般以苯并杂环代替嘌呤环或嘌呤环上取代基进行结构变化 ,脲素细胞分裂素结构改造 ,通常是改变 N-取代基的化学结构 ,为寻找化学结构更类似天然植物细胞分裂素的化合物 ,在合成 N-取代苯基 -N′-( 6-苯…     

Synthesis and Antibacterial Activities of 4—Amino—3—（1—aryl—5—methyl—1,2,3—triazol—4—yl）—5—mercapto—1,2,4—triazoles／2—Amino—5—（1—aryl—5—methyl—1,2,3—triazol—4—yl）—1,3,4—

Treatment of 4-amino-3-(1-aryl-5-methyl-1,2,3-triazol-4-yl)-5-mercapto-1,2,4-triazoles/2-amino-5-(1-aryl-5-methyl-1,2,3-triazole-4-yl)-1,3,4-thiadiazoles with benzaldehyde,acetone and ω-bromoacetophenone was tested and compared.The title compounds Schiff bases,amides,imidazolo [2,1-b]-1,3,4-thiadiazoles and 7H-s-triazolo[3,4-b]-1,3,4-thiadiazines have been confirmed by elemental analyses,^1H NMR,IR and MS spectra.All the compounds have also been screened for their antibacterial activities against B.subtilis,S.aureus and E.coli.     

SYNTHESIS AND MOLECULAR STRUCTURE OF METHYL 1—BENZYL—6—PHENYLPIPERIDIN—2—ONE—5—CARBOXYLATE

<正> C20H21NO3,Mr=323.39,monoclinic, space group P21, a= 7. 338(2), b=15. 419(3),c=7. 515(1)A,β=95.98(1)°,V= 845. 7(2)A3,Dm(flotation in aq. KL)=1.267,Dx(Z=2)=1.270gcm-3,λ(MoKα)=0.71069A,μ=0.08cm-1,F(000)=344,T=295°K,final RF=0. 042 for 1651 observed reflections. The title compound was synthesized and established as the trans isomer, with the phenyl and carbomethoxy substituents occupying pseudo-axial and axial positions, respectively, of the piperidin-2-one ring in a half-chair conformation.     

3,5—环—6—甲氧基—孕甾—20（22）—烯立体选择性硼氢化反应的研究

3,5-环-6-甲氧基-孕甾-20S-22-醇1 是合成2的前体,而后者是合成高效植物激素油菜甾醇内酯3及其类似物的关键中间体.     

A New Method for Synthesis of Methyl 3—Azido—3—deoxy—2—O—mesyl—5—O—benzoylxylofuranoside

A new method for synthesis of 3-azido-3-deoxyxylofuranoside was described. D-ribose was methylated, then treated with methanesulfonyl chloride to give Ⅱ.Ⅱ was selectively replaced by benzoate at the 5-position to give Ⅲ. All these processes gave good yields. Ⅲ was treated with sodium azide to afford Ⅳ, whose structure was determined by ^1H NMR and ^13C NMR.     

开链冠醚类似物研究Ⅴ．4－氧硫代安替比林为端基的开链冠醚等效物的合成

合成并鉴定了１０种以４－氧硫代安替比林为端基的开链冠醚类似物。报道了４－氧安替比林硫羰基化的新方法。     

A New Solution—phase Parallel Synthesis of 2—Alkyamino—3—aryl—5—phenylmethylene—3,5—dihydro—4H—imidazol—4—ones

Thirteen new 2-alkylaminoimidazolones(4) wre rapidly synthesized by a new solution-phase parallel synthetic method,which includes aza-Wittig reaction of iminophosphorane(1) with aromatic isocyanate to give carbodi-imide(2) and subsequent reaction of 2 with various aliphatic primary amine in a parallel fashion.The products were confirmed by ^1H NMR,MS,IR and X-ray crystallographic analysis.The unusual selectivity of the cyclization was probably due to the deometry of the guanidine intermediate.     

Synthesis of 3—Biaryl—1—ferrocenyl—2—propene—1—ones

The novel structures of organometallic compounds 3-biaryl-1-ferrocenyl-2-propene-1-ones 5 were synthesized for nonlinear optical chromophores by Suzuki cross-coupling reaction.Their structures were determined with elemental analyses,^1H NMR spectra and ^13C NMR spectra.     

克力托辛(Clitocine)及其类似物的合成与生物活性

克力托辛是一种从蘑菇Clitocybe inversa中分离出的天然核苷.它及其类似物具有很高的生物活性.综述了克力托辛及2'-脱氧克力托辛类似物、碱基修饰克力托辛类似物、5'-脱氧克力托辛类似物、碳环克力托辛类似物以及无环克力托辛类似物的合成方法,并对克力托辛及其类似物在农业害虫杀灭、腺苷激酶抑制剂、抗肿瘤、抗病毒等药物研究中的应用进行了概述.     

稀土—5—Br—PADAP螯合物的高效液相色谱分离与测定

以配合物形式分离金属离子已有报道.胡之德等研究了In、Pt、Pd等金属与5-Br-PADAP螯合物的色谱行为,在硅胶柱上成功地分离了这几种金属元素.林长山等应用反相高效液相色谱法,分离了Fe(Ⅲ)、Co(Ⅱ)和V(Ⅱ)3种金属的5-Br-PADAP螯合物,并做了定量的研究.本文应用高效液相色谱法研究了镧系-5-Br-PADAP螯合物色谱行为,探讨了相关因素对分离和测定的影响,讨论了螯合物的保留值与稀土元素原子半径的关系.     

右旋肌醇甲醚腺嘌呤核苷类似物的合成

以右旋肌醇甲醚为原料,经保护的甲烷磺酸酯与腺嘌呤缩合,合成了腺嘌呤核苷类似物5.此外,化合物3经酸水解,再经环氧化高产率地合成了重要的中间体7,腺嘌呤在强有机碱存在下,对环氧化合物7进行区域性的开环反应,合成了另外两种腺嘌呤核苷类似物8和9.     

用二氧化硫脲合成4—甲基—4‘—氨基二苯醚的研究

4甲基4′氨基二苯醚是合成农药、染(颜)料、医药的重要中间体.传统的制备方法是由4 甲基4′硝基化合物(简称硝基物)在盐酸存在下用二氯化锡还原得到[1] ,该方法工艺成熟、产品质量好,但产率低,污染严重.陈其亮等报道了由硝基物催化加氢的方法[2],但存在设备投资大,操作繁锁等缺点.二氧化硫脲(Thiourea dioxide ,简称TD)是一种非常优良的还原剂,已广泛应用于有机合成的许多方面[3,4],但应用于标题化合物的制备未见报道,本文对此进行了研究,收到较好效果.合成路线如下:     

On the Mechanism of Condensation between 5—Amino—4,6—dichloro—2—methylpyrimidine and 1—Acetyl—2—imidazolin—2—one

The condensation reaction between 5-amino-4,6-dichloro-2-methylprimidine and 1-acetyl-2-imidazolin-2-one using POCl3 as solvent gave 4,6-dichloro-2-methyl-5-(1-acetyl-tetra-hydro-imidazo-2-ylidene)-aminopyrimidine predominantly and 4,6-dichloro-2-methyl-5-{1-1-(2-oxo-tetrahydro-imidazolyl)]-acetene}-aminopyrimidine as by-product. No 4,6-dichloro-2-methyl-5-(1-acetyl-2-imidazolin-2-yl)-aminopyrimidine was found. The result indicated an esterifi-cation-addition-elimination mechanism.     

新型烟酰胺腺嘌呤二核苷酸(NAD)类似物的合成及其辅酶活性

尝试4种形成焦磷酸键的方法合成了5种结构新颖的新型烟酰胺腺嘌呤二核苷酸(NAD)类似物.初步考察了类似物的生物活性,发现苹果酸酶和醇脱氢酶以类似物3b和3d为辅酶时,活性只有以NAD为辅酶时的13%～30%;而以类似物3a,3c和3e为辅酶时,这些酶的活性均极低.     

Synthesis of 5—Aryl—1,2—dihydro—1—pyrrolizinones

In order to search for new potent anti-inflammatory and analgesic agents in pyrrolizinones,the title compounds were designed and synthesized.A series of the compounds were prepared with two different synthetic schemes.Some of the compounds showed remarkable anti-inflammatory and/or analgesic activities on mice.     

Synthesis and Biological Activities of 3—（2—Furyl）—4—aryl—1,2,4—triazole—5—thiones

A series of novel compounds 3-(2-furyl)-4-aryl-1,2,4-triazole-5-thiones have been synthesized.All the compounds were characterized by spectral data and elemental analysis. The preliminary biological test showed that some of them exhibited excellent plant-growth regulative activities.     

Crystal and Molecular Structure of N—Phenyl 1—Methoxycarbonylmethyl—3—benzyl—1,2,3,4—tetrahydro—4—oxo—1,3,2—benzodiazaphosphorin—2—thiocarboxamide 2—Oxide

1 INTRODUCTIONOrganophosphorus compounds are ubiquitous in nature and they have broad applications in the fields of agriculture and medicine. During the past two decades, (-ketophosphonates and their derivatives containing sulfur have attracted considerable attention because these compounds are endowed with special physical, chemical and pharmacological properties due to the proximity of the carbonyl and the phosphoryl groups[1～8]. In the study on new pharmacenticals and agrochemicals, th…     

Crystal Structure of 5—（l—Menthyloxy）—3—chloro—4— Pyrrolidinyl—2（5H0—f

The molecular structure of the title compound 5-(l-menthyloxy)-3-chloro-4-pyrrolidinyl-2(5H)-furanone, C18H28ClNO3(Ⅰ), has been determined by X-ray diffraction at 296(1)K. The crystal is monoclinic with space group P21, a=9.457(3), b=10.413(3), c=9.525(2), β=95.19(2)°, V=934(1) 3, Z=2, Mr=341.88, Dx=1.22 g/cm3, μ=2.15 cm-1, F(000)=368. The final R factor is 0.059, and Rw is 0.065 for 1020 observed reflections with I≥3σ(I). The absolute configuration at C(14) of the acetal carbon was proved to be S, taking into account the known configuration of 1R, 2S, 5R-menthyl moiety. There are three rings in the molecule of this compound: the furanone ring, the pyrrolidine ring and the mentholoxy group ring. The franone ring is connected with the pyrrolidine ring and the mentholoxy ring by N atom and μ2-O bridge atom respectively.