1-benzoyl-2-(2-naphthyl)-selenourea

During our synthesis of N-benzoyl-N'-aryl selenourea derivatives, we isolated the title compound. One of them was selected optically for the diffraction study. The crystal belongs to the Monoclinic space group P21/n, Mr = 353.27, a = 11.073(1)? , b = 5.745(1) ?, c = 24.356(5) ?, β = 92.10 (1) , V = 1548.3 (4) ?3, Z = 4, Dx=1.515 Mg/m3,λ(Mo Kα)=0.71073 ?,θ = 1.67-25,μ o = 2.428 mm-1 , T = 296 (2) K. View of the molecule showing the labeling of the non-H atoms are described as: The se…     

Synthesis of Two Isomeric Tetrasaccharides 0-α-L-Fucopyranosyl-(1→3) and (1→4)-0-(2-Acetamido-2-Deoxy-β-D-Glucopyranosyl)-(1→3)-0-(β-D-Galactopyranosyl)-(1→4)-D-Glucopyranose and a Related Tetrasaccharide 0-α-L-Fucopyranosyl-(1→3)-0-(2-Acetamido-2-Deoxy-β-D-Glucopyranosyl-(1→6)-0-(β-D-Galactopyranosyl)-(1→4)-D-Glucopyranose

ABSTRACT

Synthesis of three tetrasaccharides, namely, 0-α-L-fucopyranosyl-(1→3)-0-(2-acetamido-2-deoxy-β-D-glucopyranosyl)-(1→3)-0-(β-D-galactopyranosyl)-(1→4)-β-D-glucopyranose (7), 0-α-L-fucopyranosyl-(1→4)-0-(2-acetamido-2-deoxy-β-D-glucopyranosyl)-(1→3)-0-(β-D-galactopyranosyl)-(1→4)-D-glucopyranose (9), and 0-α-L-fucopyransoyl-(1→3)-0-(2-acetamido-2-deoxy-β-D-glucopyransoyl)-(1→6)-0-(β-D-galactopyranosyl)-(1→4)-D-glucopyranose (15) has been described. Their structures have been established by ¹³C NMR spectroscopy.     

Synthesis,Structure and Biological Activities of 2-(1H- 1,2,3-Benzotriazol-1-yl)-1-(4-methylphenyl)-2- (1H-1,2,4-triazol-1-yl)-1-ethanone

IntroductionTriazole derivatives have become the most rapidlyexpanding group of antifungal compounds with advanta-ges of lowtoxicity, high oral bioavailability and broad-spectrum antifungal activity, which can be used againstfungi including most yeasts an…     

Synthesis of 2-(3-hydroxy-2-methyl-1-alkenyl)-1-pyrrolines and 2-(3-hydroxybutyl)-1-pyrroline using α-lithiated 2-methyl-1-pyrroline

Condensation of 2-methyl-1-pyrroline with chloroacetone or 3-chloro-2-butanone using LDA in THF afforded novel 2-(3-hydroxy-2-methyl-1-alkenyl)-1-pyrrolines via a peculiar reaction mechanism instead of the anticipated 2-(3-oxobutyl)-1-pyrrolines. The intermediacy of 2-(2,3-epoxy-2-methylalkyl)-1-pyrrolines in the latter transformation was demonstrated by immediate reductive epoxide ring opening utilizing lithium aluminium hydride in diethyl ether. Furthermore, 2-(3-oxobutyl)-1-pyrroline was prepared via an alternative approach through alkylation of 2-methyl-1-pyrroline with 3-chloro-2-(methoxymethyloxy)-1-propene using LDA in THF, followed by acid hydrolysis. Reduction of 2-(3-oxobutyl)-1-pyrroline by sodium borohydride in methanol afforded the corresponding 2-(3-hydroxybutyl)-1-pyrroline in good yield.     

2-苯基-1-(4-(1-吡咯乙氧基)苯基)乙酮的合成

2-苯基-1-(4-(1-吡咯乙氧基)苯基)乙酮是合成抗骨质疏松药拉索昔芬重要的结构片段。以苯酚为原料经成醚,磺酰氯酯化得到磺酸酯,然后经亲核取代反应,傅-克酰基化反应高收率地合成了目标化合物,其结构通过NMR和HRMS进行了表征。     

(S)-1-(2-氯乙酰基)吡咯烷-2-甲酸的制备及晶体结构

以L-脯氨酸和氯乙酰氯为原料合成维格列汀的重要中间体(S)-1-(2-氯乙酰基)吡咯烷-2-甲酸(1)。甲醇体系室温挥发14 d培养得到1的无色透明块状晶体，通过单晶X-射线衍射技术对其进行结构解析。结果表明1晶胞属于正交晶系，P2₁2₁2₁空间群，分子式为C₇H₁₀NO₃Cl，相对分子质量为191.61 g/mol，立体构型和预测构型一致，确证了1的空间结构。      

微乳液-1-(2-吡啶偶氮)-2-萘酚体系测定Cd(Ⅱ)

研究了Ｏ／Ｗ型阴离子微乳液十二烷基硫酸钠（ＳＤＳ）／正丁醇（ｎ－Ｃ４Ｈ９ＯＨ）／正庚烷（ｎ－Ｃ７Ｈ１６）／Ｈ２Ｏ对Ｃｄ（Ⅱ）与１－（２－吡啶偶氮）－２－萘酚（ＰＡＮ）显色体系的增敏增稳作用,试验结果表明,其灵敏度为ε＾５４５＝１．９３＊１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１,与相同含水量的ＳＤＳ胶束体系（ε＾５４５＝１．１５＊１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１）比较,其测定灵敏度显著增加,用于香烟样品分析,结果满意。     

Comeplexes of 1-(2′-hydroxybenzyl)-2-(2′-hydroxyphenyl)-benzimidazole with U(VI) and Ce(IV)

Some new U(VI) and Ce(IV) complexes of 1-(2′-hydroxybenzyl)-2-(2′-hydroxyphenyl)-benzimidazole have been prepared and characterized by spectrg magnetic and conductance studies. IR spectral data suggests that the ligand in all the complexes is monodenate through the tertiary nitrogen and that the phenolic oxygen is free from coordination. Conductivity measurements indicate that the nitrate and acetate complexes of U(VI) are non-electrolytes, whereas the nitrate complex of Ce(IV) is a 1:1 electrolyte.     

Das 1-(4-Hydroxyphenyl)-1-hydroxy-2-n-butylamino-?thansulfat (Vasculat)

Ohne Zusammenfassung     

2-(1H-咪唑-1基)-1-(2,3,4-三甲氧基苯)乙酮的和成

联苯三醚;制备;2-(1H-咪唑-1基)-1-(2;3;4-三甲氧基苯)乙酮的和成     

(Z)-2-(1H-咪唑-1-基)-1-(2,3,4-三甲氧基)苯乙酮肟酯的设计与合成

三甲基苯乙酮肟;立体异构体;(Z)-2-(1H-咪唑-1-基)-1-(2;3;4-三甲氧基)苯乙酮肟酯的设计与合成     

(S)-1-[2-(3-羟基金刚烷-1-氨基)乙酰基]吡咯烷-2-甲酰胺的合成

为了对维格列汀进行质量控制,合成了其相关物质:(S)-1-[2-(3-羟基金刚烷-1-氨基)乙酰基]吡咯烷-2-甲酰胺(1)。本文以L-脯氨酸和盐酸金刚烷胺为原料,经仲N-氯乙酰化,酰胺化,氨基取代3步反应合成,合成的物质其结构经MS、1H-NMR和13C-NMR确证,纯度经HPLC检测亦符合国家药品生物制品检定所的规定。应用星点设计-效应面法优化工艺后,提高了其收率和纯度,具有重要的应用价值。     

微乳液--1-(2-吡啶偶氮)-2-萘酚体系测定Co(Ⅱ)

The spectrohpotometric determination of Co(Ⅱ) was studied with 1-( 2 -pyridylazo)-2-naphthol in the sodium dodecyl sulphate/n-heptane/water micr oemulsion medium.The apparent molar absorptivity is 1.84×10⁴ L^.mol -1^.cm^-1 at 575 nm.Beer's law is obeyed in the range of 0～ 50 μg/25 mL for Co(Ⅱ).     

2-(2-(5-氟尿嘧啶-1-基)乙酰氨基)丙酸的合成及表征

以5-氟尿嘧啶-1-基乙酸为原料,N,N-二异丙基碳二亚胺(DIC)/1-羟基苯并三氮唑(HOBt)为缩合剂,分别与L-丙氨酸甲酯和D-丙氨酸甲酯通过液相偶联合成了(S)-和(R)-2-(2-(5-氟-2,4-二氧-3,4-二氢嘧啶-1(2H) -基)乙酰氨基)丙酸甲酯对映体,收率分别为82％和80％;室温下将化合物水...     

DiastereoselectiveandEnantioselectiveSynthesisof(1S,2S)-2-Ethyl-1-aminocyclopropaneCarboxylicAcid

During the last decade, 1-aminocyclopropanecarboxylic acid and its derivatives (ACCS) have attracted increasing attention of organic and bioorganic chemists due to their outstanding biological properties, ranging from antimicrobial, insecticidal, plant growth and fruit ripening controls, etc.1. Moreover, the three-membered carbocycle provides building blocks of unprecedented synthetic potential because it undergoes selective ring opening, ring enlargement or cycloaddition reactions2. The mo…     

(2S)-(+)-2-溴-1-(6'-甲氧基-2'-萘基)丙-1-酮的不对称合成

以(2R,3R)-酒石酸二甲酯为手性辅助剂,6-甲氧基-2-丙酰基萘经缩酮化、溴化铜不对称溴化、水解等反应合成了(2S)-2-溴-1-(6'-甲氧基-2'-萘基)丙-1-酮。总收率94%。     

Synthesis of propyl O-(α-L-rhamnopyranosyl)-(1→3)-[2,4-di-O-(2s-methylbutyryl)-α-L-rhamno-pyranosyl]-(1→2)-(3-O-acetyl-β-D-glucopyranosyl)-(1→2)-β-D-fucopyranoside,the tetrasaccharide moiety of Tricolorin A

Propyl O-(α-L-rhamncpyranosyl)-(1→3)-[2,4-di-O-(2s-methylbutyryl)-α-L-rham-nopyranosyl]-(1→2)-(3-O-acetyl-β-D-glucopyranosyl)-(1→2)-β-D-fucopyranoside (1), the tetrasac-charide moiety of Tricolorin A, was synthesized in total 23 steps with a longest linear sequence of 10 steps, and overall yield of 3.7% from D-Glucose. The isomerization of the dioxolane-type berzyli-dene in the presence of NIS/AgOTf was observed. Tetrasaccharide 1 exhibited no activity against the cultured P388 cell as Tricolorin A did.     

1-(吡啶-2-基)-2-芳氧基-2-(α-1H-1,2,4-三唑-1-基)乙酮的合成、晶体结构与生物活性

为了从三唑类化合物中寻找新的活性化合物,采用活性亚结构拼接和活性叠加方法,将吡啶环结构单元引入到三唑类化合物分子中,制备了一系列未见文献报道的新型含吡啶环结构的三唑类衍生物.经1H NMR,13C NMR,IR,MS和元素分析对所合成的化合物的结构进行了表征.此外,采用X射线单晶衍射分析方法进一步测定了化合物4k的晶体结构.初步的生物活性测试表明,部分目标化合物在试验浓度下具有一定的杀菌和植物生长调节活性.     

Synthesis of 1-[6-Fluoro-(2S)-3H,4H-dihydro-2H-2-chromenyl]-(1R)-1,2- ethanediol and 1-[6-Fluoro-(2R)-3H,4H-dihydro-2H-2-chromenyl]- (1R)-1,2-ethanediol

Benzopyran compounds possess diverse pharmacological properties such as β-blockade, anticonvulsant and antimicrobial.[1,2] Our interest has been focused on the synthesis of 1-[6-Fluoro-2S]-3H,4H-dihydro-2H-2-chromenyl]-(1R)-1,2-ethanediol (6) and 1-[6-fluoro-(2R)-3H,4H-dihydro-2H-2-chromenyl]-(1R)-1,2-ethanediol (7) which are particularly convenient precursor to (S,R,R,R)-NE (8). 8 containing four asymmetrical carbon atoms was reported to be the most active isomer.[3] Chandrasekhar[4] has reported on the synthesis of 8. The key step to synthesize this compound is to obtain the chiral chromanone 6 and 7. 6 was accomplished in 8 steps by the Clasien rearrangement and a one-pot Sharpless asymmetric epoxidation, but the compound 7 was accomplished in 10 steps. Johannes[5] used Zr-catalytic kinetic resolution of allylic ethers and Mo-catalyzed chromene formation to synthesize 8 in 14 steps. However both of the methods request many synthetic steps and expensive reagents.     

3,4-二氢-1-(4-哌啶基)-2(1H)-喹啉酮的合成

以苄胺为原料,经6步反应得到新型抗高血压药OPC-21268的中间体3,4-二氢-1-(4-哌啶基)-2(1H)-喹啉酮,总收率13．9％．