A Novel Fused Phosphorus Heterocycle: 4-(1′, 2′, 3′, 4′-Tetrahydro- 1, 3, 2-benzodiazaphosphorin-2′-sulfide)-3, 4b, 4a- thiazphosphaphenanthridine Derivative

The first example of fused phosphorus heterocyclic 4-[ l′-(β-bromoethyl)-4'-oxo-3'-prop yl-1′, 2′, 3′, 4-tetrahydro-1, 3, 2-benzodiazaphosphorin-2′-sulfide]-1, 2, 3, 4, 4a, 4b, 5, 6-octahydro -6-oxo-5-propyl-3, 4b, 4a-thiazphosphaphenanthridine 4a, 2′-dioxide was synthesized in excellent yield by refluxing a mixture of 1-(2-bromoethyt)-2, 3-dihydro-3-propyl-l, 3, 2-benzodiazaphos phorin-4(1H)-one 2-oxide with carbon disulfide in benzene in the presence of triethylamine.     

1-(2′,2′,2′-Trifluoroethyl)-4-phosphopyrazoles: Synthese et Etude Spectroscopique ir et RMN 1H, 13C, 19F,et 31P

Seven new 1-fluorinated-4-phosphopyrazoles 2 have been prepared in 60–94% yield by cyclization of N-(2′,2′,2′-trifluoroethyl) phosphonyl β-hydrazones 1 with triethyl orthoformate in the presence of acetic acid. The IR data, the ¹H, ¹³C, ¹⁹F, ³¹P chemical shifts and coupling constants of the compounds 2 are reported.     

N,N,N′,N′,-(四环己基-3-氧戊烷)二酰胺的晶体结构

双酰胺开链冠醚由于合成方便,络合性能好而引起人们的兴趣.Simon等合成了N,N,N′,N′-(四环己基-3-氧戊烷)二酰胺和它的Ca~(2 ),Mg~(2 )络合物,但未见关于配体晶体结构的报道.我们开展了有关这类化合物的合成及应用研究.本文报导标题化合物的晶体结构.     

2′,4-二羟基-4′,6′-二甲氧基-二氢查尔酮的首次全合成

以2,4,6-三羟基苯乙酮和对羟基苯甲醛为起始原料,经选择性的甲基化,甲氧甲基化,羟醛缩合,还原,脱保护等反应首次完成了2′,4-二羟基-4′,6′-二甲氧基-二氢查尔酮(1)的全合成,总收率40%。1和中间体的结构经1HNMR,IR和MS表征。     

Synthesis and antiviral evaluation of 2′,2′,3′,3′-tetrafluoro nucleoside analogs

Herein, we report the synthesis of novel 2′,2′,3′,3′-tetrafluorinated nucleoside analogs along with their phosphoramidate prodrugs. A tetrafluoro ribose moiety was coupled with different Boc/benzoyl-protected nucleobases under Mitsunobu conditions. After deprotection, tetrafluorinated nucleosides 13b, 14b, 20b-22b were reacted with phenyl-(isopropoxy-l-alaninyl)-phosphorochloridate to afford corresponding monophosphate prodrugs 24b–28b. All synthesized compounds were evaluated against several DNA and RNA viruses including HIV, HBV, HCV, Ebola and Zika viruses.     

Stereoselective synthesis and absolute configuration of (1′R,3R,4R)-4-acetoxy-3-(2′,2′,2′-trifluoro-1′-hydroxyethyl)azetidin-2-one

The title compound 3, an intermediate in the synthesis of fluorocarbapenems, is obtained with high stereocontrol by the condensation of (R)-(+)-ethyl 4,4,4-trifluoro-3-hydroxybutanoate with N-trimethylsilyl cinnamylidenimine. X-Ray diffraction analysis of the condensation product and chemical correlations allowed the unambiguous determination of the absolute configuration.     

由2′,4′-二氢-6′-甲氧基-3′,5′-二甲基查耳酮合成新黄酮

在DMSO/I2的氧化作用下,由2′,4′-二氢-6′-甲氧基-3′,5′-二甲基查耳酮可合成一种全新结构的黄酮:7-羟基-5-甲氧基-6,8-二甲基黄酮(产率91%),而在HCl/MeOH作用下则得到了两种黄烷酮:7-羟基-5-甲氧基-6,8-二甲基黄烷酮(产率70%)和5,7-二羟基-6,8-二甲基黄烷酮(产率20%)。     

1,2,1′,2′-双蒽醌-3,12-二羧酸二甲酯的合成

我们合成了化合物5,6,7,8,9,这些化合物的合成至今尚未见文献报道。化合物4虽然是已知化合物,但我们研究了便于实验室制备的方法。     

Complexation of the N,N′,O-donor ligand N-trans-(2′-hydroxycyclohexyl)-2-aminomethylpyridine

The potentially tridentate N,N′,O-donor N-trans-(2′-hydroxycyclohexyl)-2-aminomethylpyridine (1) forms ML₂ complexes with M(II)?=?Cu, Ni, and Zn. X-ray crystal structures of the isostructural Ni(II) and Zn(II) complexes confirm bis-tridentate coordination in significantly distorted octahedral geometries as the all-cis facial isomer. Structural comparisons with the previously reported all-trans facial Cu(II) and cis,cis,trans(N_py) facial Co(III) complexes are presented. Protonation constants for 1 and stability constants with Cu(II), Ni(II), and Zn(II) are reported, with both ML and ML₂ species defined. The trend for ML (log K ₁ values for Cu, Ni, and Zn of 8.3, 6.9, and 5.3, respectively) is conventional. Protonation and stability constants with Cu(II) for N,N-bis(2-pyridylmethyl)amine (2) were also defined. The log K ₁ value measured for 2 of 7.4 is very similar to that found for 1 of 8.3, despite the marked difference in the third donor group; it appears that the third donor of the tridentate ligand generally binds only poorly to Jahn–Teller elongated Cu(II) in solution.     

1,2,1′,2′-双蒽醌-3,12-二羧酸的还原反应

1,2,1＇,2＇-双蒽醌-3,12-二羧酸(1)是一个π-共轭体系芳环化合物,内环酮基由于受空间效应和共振效应的影响,不能被还原成相应的醇或相应的碳氢基团,却成了不常见的内“双氧桥”化合物(4)。化合物2,3,4的结构已经确定,并对1的还原机理进行了初步讨论。     

1-(2′-苯基-1′,2′,3′-三唑-4′-甲酰基)-4-芳基氨基硫脲及其环化产物的合成

以2-苯基-1,2,3-三唑-4甲酰肼为原料合成了几种新的1-(2′-苯基-1′,2′,3′-三唑-4′-甲酰基)-4芳基氨基硫脲,在不同条件下环化,制得一系列新的1,3,4-噻二唑、1,3,4- 二唑和1,2,4-均三唑衍生物.化合物的结构经元素分析、IR、1HMR和MS确证,并对其波谱性质进行了讨论.     

Synthesis and Biological Activity of Novel 2,3-Dihydro-2-phenylsulfonylhydrazono-3-(2′,3′,4′,6′-tetra-O-acetyl-β-D-glucopyranosyl)thiazoles

A series of novel 2,3-dihydro-2-phenylsulfonylhydrazono-3-(2',3',4',6'-tetra-O-acetyl-β-D-glucopyranosyl) thiazoles were designed and synthesized via the reaction of thiosemicarbazide with chloroaldehyde.Their chemical structures were characterized by 1H and 13C NMR spectroscopy and elemental analysis.The bioassay results indicate that some of these compounds exhibit moderate fungicidal and herbicidal activities.     

N,N,N′,N′-四(2-苯并咪唑亚甲基)-1,2-乙二胺的晶体和电子结构

合成了六齿配体N,N,N′,N′-四(2-苯并咪唑亚甲基)-1,2-乙二胺(EDTB).对该配体进行了元素分析、紫外和红外表征;采用X射线衍射方法测定了晶体结构,依据晶体结构数据使用G98程序对配体进行了量子化学计算.     

Synthesis and mesomorphic properties of 4-methoxyphenyl 4′- n -alkoxy-2′,3′,5′,6′-tetrafluorobiphenyl-1-carboxylates

A novel type of 4-methoxyphenyl 4′-n-alkoxy-2′,3′,5′,6′-tetrafluorobiphenyl-1-carboxylates have been synthesized. Textural observations by polarizing microscopy and DSC measurements of the phase transitions show that all of these compounds are thermotropic liquid crystals with only a nematic mesophase. The relationship between the properties and chemical structures of these compounds is discussed.     

N-取代-N′-(2′,3′,4′,6′-四-O-乙酰基-β-D-吡喃葡萄糖基）（酰）氨基硫脲的合成

利用2,3,4,6-四-0-乙酰基-β-D-吡喃葡萄糖异硫氰酸酯(I)分别和芳酰肼(Ⅱ),2-氨基-5-烷基/芳基-1,3,4-噻二唑(Ⅲ),3-烷基/芳基-4-氨基-5-巯基-1,2,4-三唑(Ⅳ),O,O-二烷基(硫代)磷酰肼(V,Ⅵ)反应,制得了目标物1a～1c,2d～2e,3f～3i,4j～4k和51等12种新化合物,IR,1H NMR和MS分析结果证明产物为β构型.     

1′-C-氰基-2′,3′,5′-三-O-苯甲酰基-β-D-呋喃胸苷的声化学合成

本文首次应用超声波技术合成了1’-C-氰基-2’,3’,5’-三-O-苯甲酰基-β-D-呋喃胸苷,反应时间1h,产率96～100％,与通常的化学合成方法相比,反应速度及产率大辐度提高。     

Transition metal(II) complexes of 1-(α-hydroxynaphthyl)-2-(3′-methyl-5′-mercapto-1′,2′,4′-triazole)-2-aza-ethane

Summary Binuclear metal complexes of the type [M(HMTE)-(H₂O)₂]₂, where HMTE=1-(-hydroxynaphthyl)-2-(3-methyl-5-mercapto-1,2,4-triazolc)2-aza-ethane and M-Cu^II, Co^II, Ni^II and Mn^II have been prepared and characterized. An octahedral geometry around the metals is proposed. The complexes have been screened as possible fungicides.     

Synthesis of Novel 1-Arylsulfonyl-4-(1′-N-2′, 3′, 4′, 6′-tetra-O-acetyl-β-D-glucopyranosyl)thiosemicarbazides

Some 1-arylsulfonylthiosemicarbazides have been reported as fungicides1 and bacterio-static agents2. Recently, it is well documented that thiosemicarbazide is a novel class ofnon-peptide antagonists for bradykinin B2 , which is beneficial in the symptomat…     

4,5-二氢咪唑并[1,2-b]-1′,2′,4′-三唑-4-酮衍生物的合成与杀菌活性

应用芳基异氰酸酯与烯基膦亚胺1的氮杂Wittig反应,得到的碳二亚胺2,再与水合肼作用得到氨基咪唑啉酮衍生物4.而后用4与芳基异氰酸酯(或酰氯)、三苯基膦、六氯乙烷和三乙胺"一锅"反应,得到4,5-二氢咪唑并[1,2-b]-1′,2′,4′-三唑-4-酮衍生物6或7.探讨了所合成新型稠杂环化合物的生物活性,结果表明部分化合物表现出良好的杀菌活性.如7c在50 mg/L浓度时,对棉花枯萎菌、稻瘟菌、黄瓜灰霉菌和油菜菌核菌的抑制率均达100%.