2-氨基取代噻唑基膦酸脂的合成

本文报导一系列2-氨基-5-取代-4-噻唑基膦酸酯和2-氨基-4-取代-5-噻唑基膦酸酯的合成. 这类化合物显示了一定的杀菌活性.     

2-氨基取代噻唑基膦酸脂的合成

本文报导一系列2-氨基-5-取代-4-噻唑基膦酸酯和2-氨基-4-取代-5-噻唑基膦酸酯的合成. 这类化合物显示了一定的杀菌活性.     

N-取代苯基N'-(6-苯并噻唑基)脲类化合物的合成

为了寻找具有植物细胞激动素活性的新化合物,以苯并噻唑和取代苯胺为原料,将取代苯脲基引入到苯并噻唑的6-位上,合成了7个N-取代苯基N'-(6-苯并噻唑基)脲类化合物,它们的结构经元素分析、IR和1HNMR确定,7个化合物的合成收率分别为74%,76%,85%,82%,70%,73%和72%.     

含苯并噻唑杂环的α-氨基膦酸二苯酯的合成及生物活性

α氨基膦酸作为氨基酸的含磷类似物,具有广泛的除草［１］、杀菌［２］和植物生长调节活性［３］．最近的研究表明,某些α氨基膦酸衍生物还具有较好的抗植物病毒活性［４,５］．在研究植物病毒抑制剂的过程中,我们发现含苯并噻唑杂环的α氨基膦酸二乙酯类化合物...     

N-[芳氧乙酰基]α-氨基膦酸二苯酯的合成

通过取代芳氧乙酸与α－氨基膦酸二苯酯的缩合反应合成了12个未见报道的目标化合物，用元素分析，IR，^1H NMR确定了化合物的结构。     

α-氨基膦酸及其酯的绿色合成研究进展

作为氨基酸的类似物,α-氨基膦酸及其酯不仅在化学和农药学方面有重要的作用,在医学上也有很广阔的应用前景,因此,人们对其合成方法进行了很多研究。本文综述了近年来对α-氨基膦酸及其酯的绿色合成研究的工作,并对其发展趋势作了进一步的展望。     

新型光学活性α-氨基磷酸及其酯合成进展

α-氨基膦酸酯是一类很重要的天然氨基酸类似物，具有新颖的化学结构和多 种生理活性。综述了近年来光学活性α-氨基膦酸及酯的合成进展。     

N-(烷氧羰基或烷氧羰甲基-烷氧膦酰基)-α-氨基膦酸二苯酯的研究

以膦酰甲酸(PFA)及其同系物膦酰乙酸(PAA)为先导化合物,利用膦酰氯与α-氨基膦酸酯在碱存在下反应,将α-氨基膦酸酯引入PFA及PAA中,使其N-端与膦原子相连,合成了化合物Ⅰ和Ⅱ.研究了产物的~(31)PNMR,发现当R~3为烷基时~3J_(pp)较R~3为(取代)苯基时小,并对其进行了讨论.同时测定了产物的生物活性,部分化合物具有良好的抑制植物烟草花叶病毒(TMV)活性,抑制率超过对照药剂DHT(2,4-二氧六氢-1,3,5三嗪),部分化合物还具有一定的抑制癌细胞活性.I:n=0,R~1,R~2=MeO.MeO.或R~1=i-RrNH,R~2=OMe;R~3=alkyl,(substituted)PhII:n=1,R=H,Me;R~1,R~2,R~3同上.     

光学活性α-氨基膦酸及其酯的不对称合成

综述了近年来光学活性α－氨基膦酸及其酯的各种不对称合成方法,包括化学计量不对称合成和催化不对称合成。重点介绍了近年发展起来的催化不对称合成方法,并且对各种合成方法的优劣进行了评述。     

N-取代苯基-N′-[6-(2-甲基苯并噻唑)基]脲类化合物的合成

以 2 -甲基苯并噻唑和取代苯胺为原料 ,合成了 7个 N-取代苯基 -N′-[6-( 2 -甲基苯并噻唑 )基 ]脲类新化合物 ,产率分别为 82 .0 % ,88.5% ,87.0 % ,90 .5% ,91 .0 % ,83.5%和 85.0 %。其结构经元素分析、IR和1 H NMR确定。     

N-(2-吡咯甲酰基)氨基酸甲酯的合成

在室温条件下,氨基酸甲酯和2-三氯乙酰基吡咯经酰基化反应,以80.3%～95.6%的产率合成了系列N-(2-吡咯甲酰基)氨基酸甲酯,通过1H NMR,IR,MS和元素分析对其结构进行了表征.     

聚2-甲氧氨基-2-(2-氨基噻唑)-4-乙酸修饰电极对多巴胺、尿酸与亚硝酸盐的同时测定

采用循环伏安法(CV)将2-甲氧氨基-2-(2-氨基噻唑)-4-乙酸(AMTA)聚合修饰在玻碳电极(GCE)表面,制备了聚2-甲氧氨基-2-(2-氨基噻唑)-4-乙酸修饰的玻碳电极(PAMTA/GCE)。在pH 7.0的生理性磷酸盐缓冲溶液(PBS)中,PAMTA/GCE不仅能很好地改善多巴胺(DA)、尿酸(UA)和亚硝酸根(NO-2)的电化学行为,而且能将三者的混合液在裸GCE上重叠的弱氧化峰分成3个灵敏的氧化峰,故该修饰电极可用于对混合液中DA、UA和NO-2的同时测定。在优化实验条件下,DA、UA和NO-2的差分脉冲伏安峰电流与其浓度分别在0.3~75、1~480、20~1 680μmol/L范围内呈良好的线性关系,相关系数分别为0.989 9、0.957 1和0.992 7,检出限(3δ)分别为0.05、0.10、0.30μmol/L。将PAMTA/GCE应用于尿液和血清样本中DA、UA和NO-2的同时测定,结果满意。     

R(-)四氢噻唑-2-硫酮-4-羧酸对D,L-氨基酸酯拆分的研究

以新手性拆分试剂R(-)四氢噻唑-2-硫酮-4-羧酸[简称R(-)TTCA]对D,L-氨基酸酯进行手性拆分,分别得到(R)TTCA氨基酸酯盐1a_1f([α]_D²⁰＝-30.40°～-42.70°)及光学活性氨基酸酯2a-2f,其光学纯度为35.4%～75.8%.由1a_1f在碱存在下分解出2a-2f的对映体3a-3f,光学纯度为39.50%～69.10%.用半经验的量子化学PM3方法研究了氨基的碱性、中间产物铵盐生成热和稳定性.     

(R)-2-硫代四氢噻唑-4-羧酸及其酯的合成

L-半胱氨酸盐酸盐与二硫化碳, 氢氧化钠在硝酸铅存在下进行成环反应得到(R)-四氢噻唑-2-硫酮-4-羧酸产率76% , 后者与 醇在硫酸铁水合物催化下反应得到(R)-四氢噻唑-2-硫酮-4-羧酸酯, 产率40～82% .     

Synthesis of Novel New 2-(2-(4-((3,4-Dihydro-4-oxo-3-aryl quinazolin-2-yl)methyl)piperazin-1-yl)acetoyloxy)-2-phenyl Acetic Acid Esters

Stereoselective diazotization of (S)-2-amino-2-phenyl acetic acid (L-phenyl glycine) (4) with NaNO₂ in 6% H₂SO₄ in a mixture of acetone and water gave optically pure (S)-2-hydroxy-2-phenyl acetic acid (L-mandelic acid) (5). Esterification, gave (S)-2-hydroxy-2-phenyl acetic acid esters (6). The latter was treated with chloroacetyl chloride in the presence of triethylamine (TEA) in dichloromethane (DCM) to yield (S)-2-chloroacetyloxy phenyl acetic acid ester (2). In another sequence, the reaction of 2-(chloromethyl)-3-arylquinazolin-4(3H)-one (9) treated with N-Boc piperazine, followed by deprotection of the Boc group, to obtain 3-aryl-2-((piperazin-1-yl)methyl) quinazolin-4(3H)-one (3). Reaction of 2 with 3 in the presence of K₂CO₃ and KI gave the title compound, 2-(2-(4-((3,4-dihydro-4-oxo-3-arylquinazolin-2-yl)methyl)piperazin-1-yl) acetoyloxy)-2-phenyl acetic acid esters (1). The structures of all the new compounds obtained in the present work are supported by spectral and analytical data.     

(R)-2-甲基-7-炔-辛酸的合成

以1,5-戊二醇为起始原料,用Evans手性助剂诱导的烷基化反应构造了C-2手性中心,用Ohira-Bestmann试剂制备了末端炔基,通过13步反应,合成了(R)-2-甲基-7-炔-辛酸,总收率为17.1%,e.e.值大于99%.     

One-Pot Synthesis and Methylation of 3-[2-(1H-Benzimidazol-2-yl-Sulfanyl)-Acetyl]-Chromen-2-Ones

Abstract

3-(2-Bromoacetyl)coumarins (I), when treated with 2-mercatobenzimidazole (II) in acetone containing K₂CO₃ (mild base) and tetrabutylammonium bromide (TBAB) as a phase transfer catalyst, at room temperature yielded the title compound 3-[2-(1H-benzimidazole-2-yl-sufanyl)-acetyl]-chromen-2-one (III) in a one-pot synthesis. Alternatively, III could also be prepared by treating dithiocarbonic acid O-ethyl ester, S-[2-oxo-2-(2-oxo-2H-chromen3-yl)-ethyl] ester (V), with o-phenylenediamine (VI). The methylation of the title compound III was performed with dimethyl sulfate (DMS), in acetonitrile containing TBAB and K₂CO₃ at room temperature, resulting in 3-[2-(N-methyl-benzimidazol-2-yl-sulfanyl)]-acetyl-chromen-2-ones (VII). Alternatively, methylation of III could also be performed with DMS in acetonitrile containing K₂CO₃ as base and clay as surface catalyst. All the compounds were synthesized in good yields and their structures were confirmed by spectral and analytical data.

[Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental resource: ¹H NMR of IIIB, VB and VIIB]     

The Synthesis of Some Novel N-[a-(Isoflavone-7-O-)Acetyl ] Amino Acid Derivatives

A series of novel N-[(α)-(isoflavone-7-O-)acetyl] amino acid methyl esters were prepared from the efficient and regioselective alkylation of isoflavones with chloroacetyl amino acid derivatives under mild condition.     

Synthesis and Crystal Structure of 4-（4,6-dimethoxyl -pyrimidin-2-yl）-3-thiourea Carboxylic Acid Methyl Ester

1 INTRODUCTION Pyrimidinyl thioureas have been studied for many years because of their broad antibiosis and sterilibza- tion properties. Recent years’ study shows that pyri- midinyl thioureas not only can be used to kill insects and adjust plant growth, but also have anti-viral ac- tivities[1, 2]. From our early quantum study on these compounds, we find that they have several active cen- ters and can form polyligand complexes with metals easily[3]. These complexes are widely used as ant…