8′-溴-次黄嘌呤核■酸(8′-Br-IDP和8′-Br-IMP)的分离纯化及其鉴定

次黄嘌呤核苷二磷酸(5′-IDP)是合成“干扰素”诱导剂聚肌胞(Poly I:C)的主要原料之一。为了合成供示踪研究用的氚标记聚肌胞,我们制备了氚标记次黄嘌呤核苷二磷酸(8′-~3H-IDP);而获得层析纯的8′-溴-次黄嘌呤核苷二磷酸(8′-Br-IDP)则是首要前提。     

7，8，7′，8′-四氢番茄红素的合成

以金合欢醇为起始原料，制备了金合欢基季磷盐（3）；3与2，7-二甲基-2，4，6-辛三烯-1，8-二醛发生双分子Wittig反应合成了7，8，7′，8′-四氢番茄红素，总产率64．2％。其结构经UV，^1H NMR，IR和MS表征。     

5，8，5′，8′-二甲氧基-3，3′-二亚甲基-2，2′-双喹啉的合成

2-氨基-3,6-二甲氧基苯甲醛与1,2-环己二酮发生Fried lander缩合反应合成了新化合物5,8,5,′8′-二甲氧基-3,3′-二亚甲基-2,2′-双喹啉,其结构经UV,1H NMR,IR和MS表征。     

Synthesis and properties of 8-phenylindolo-3,3′-trimethinecyanines

The condensation of 1-methyl-2-aryl-3-(2-benzoylvinyl)indoles with substituted indoles in acetic anhydride in the presence of a mineral acid afforded 8-phenylindolo-3,3-trimethinecyanines. Their spectral, polarographic, and photographic properties were studied.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 499–501, April, 1992.     

Enantioselective imine Michael reaction for the preparation of the (8′R,8a′S)-8,8a′-dimethyl-1′,3′,4′,7′,8′,8a′-hexahydrospiro[1,3-dioxolane-2,2′(6′H)naphthalen]-6′-one building block. A formal synthesis of (+)-valencenol

The enantioselective Michael addition of a chiral imine of 4-protected 2-methylcyclohexane-1,4-dione to phenyl crotonate led after cyclization to the corresponding bicyclic lactam. Reductive cleavage of the chiral moiety followed by saponification gave the corresponding keto-acid, which was cyclized to afford a lactone. Belleau–Fujimoto reaction of the lactone then led to the title building block (diastereoselectivity 96:4, e.e. >98%) in 11% overall yield from the starting dione. (8R,8aS)-(+)-8,8a-Dimethyl-3,4,6,7,8,8a-hexahydronaphthalen-2(1H)-one was obtained after reduction of the carbonyl group, acetylation, and reductive cleavage–deprotection (52% overall yield), representing a formal synthesis of (+)-valencenol.     

Synthesis of 4′-alkyl-8-azaspiro[bicyclo[3.2.1]octane-3,2′-morpholin]-5′-ones

N-Boc-protected 8-azaspiro[bicyclo[3.2.1]octane-3,2′-oxirane] reacted with primary aliphatic amines through opening of the epoxide ring with formation of the corresponding amino alcohols which were converted into N-chloroacetyl derivatives. The latter underwent cyclization to N-Boc-protected 4′-alkyl-8-azaspiro[bicyclo[3.2.1]octane-3,2′-morpholin]-5′-ones by the action of sodium hydride in DMF, and subsequent treatment with hydrogen chloride in ethyl acetate afforded 8-azaspiro[bicyclo[3.2.1]octane-3,2′-morpholin]-5′-one hydrochlorides.     

Chelating properties of poly[5,5′-methylene-bis(8-hydroxyquinoline)-7,7′-diylethylene]

Polymeric chelates of poly[5,5′-methylene-bis(8-hydroxyquinoline)-7,7′-diylethylene] (MQE) with various metal ions have been prepared and characterized by i.r., by the measurement of metal ligand ratio, magnetic moment and electrical conductivity and by TGA. The polymeric chelates are thermally less stable than parent ligand. Ion-exchanging properties of MQE have also been studied by application of the batch equilibration method.     

A new 8-O-4′-type neolignan from Ligularia narynensis

A new 8-O-4′-type neolignan named narynenol （1） was isolated from the roots of Ligularia narynensis. Its structure and the relative configurations were confirmed by spectroscopic data interpretation. 2007 Zhong Jian Jia. Published by Elsevier B.V. on behalf of Chinese Chemical Society, All rights reserved.     

Crystal and molecular structure studies of 1′-Benzyl-8-(4-fluorobenzyl)-8-azaspiro[bicyclo-[3.2.1]octane-3,4′-imidazolidine]-2′,5′-dione

The title compound 1′-Benzyl-8-(4-fluorobenzyl)-8-azaspiro[bicyclo[3.2.1] octane-3,4′-imidazolidine]-2′,5′-dione, C₂₃H₂₃FN₃O₂ is synthesized and the structure is investigated by X-ray diffraction studies. The compound crystallizes in the triclinic crystal class in the P1 space group. The hydantoin ring adopts a planar conformation and is affected by the π conjugation. The pyrrolidine and piperidine rings in the bicyclo octane moiety adopt envelope and chair conformations respectively. The structure exhibits both inter- and intramolecular hydrogen bonds of the type N-H...O, C-H...O, and C-H...N. The oxygen atom in the hydantoin ring simultaneously accepts two hydrogen bonds to form a three-centered hydrogen bonding pattern.     

8-O-4′新木脂素化合物的不对称合成

报道了一种手性合成8—O—4′新木脂素的新方法，其中的关键步骤是以Sharpless不对称双羟化反应来构筑手性中心并以Mitsunobu反应立体选择性地构建8—O—4′新木脂素的骨架，最终以8步反应得到了天然降碳8—O—4′新木脂素的苏赤混合物，苏赤比为2：1．     

Reaction of 2′-hydroxy-1,1′: 3′,1″-terphenyl-5′-carbaldehyde with naphthalen-1-amine,quinolin-8-amine,and 1,3-diketones

Condensation of 2′-hydroxy-1,1′: 3′,1″-terphenyl-5′-carbaldehyde with naphthalen-1-amine and cyclohexane-1,3-dione, methyl 2,2-dimethyl-4,6-dioxocyclohexane-1-carboxylate, or dimedone gave the corresponding 7-(2′-hydroxy-1,1′: 3′,1″-terphenyl-5′-yl)-7,8,9,10,11,12-hexahydro-12H-benzo[c]acridin-8-ones. The reaction of 2′-hydroxy-1,1′: 3′,1″-terphenyl-5′-carbaldehyde with naphthalen-1-amine and indan-1,3-dione produced 7-(2′-hydroxy-1,1′: 3′,1″-terphenyl-5′-yl)-8H-benzo[h]indeno[1,2-b]quinolin-8-one. 7-(2′-Hydroxy-1,1′: 3′,1″-terphenyl-5′-yl)-7,8,9,10,11,12-hexahydrobenzo[b][1,10]phenanthrolin-8-ones were obtained by three-component condensation of 2′-hydroxy-1,1′: 3′,1″-terphenyl-5′-carbaldehyde with quinolin-8-amine and cyclohexane-1,3-dione, methyl 2,2-dimethyl-4,6-dioxocyclohexane-1-carboxylate, or dimedone.     

An expeditious access of 2,5′-dioxo-5′,6′,7′,8′-tetrahydro-1′H-spiro[indoline-3,4′-quinoline]-3′-carboxylate by reaction of isatin,ethyl cyanoacetate and enaminone in water

We have demonstrated three component reaction of isatin, enaminone and ethyl cyanoacetate leading to sprirooxindole scaffold without catalyst in water. The synthetic protocol has several advantages like wide substrate scope, atom-economy and operationally simple experimental procedures which provides rapid access to library of compounds. The mechanistic details of the reaction has been investigated during the course of study.     

8-5′新木脂素类化合物的合成方法研究

对羟基桂皮酸甲酯和阿魏酸甲酯分别在氧化银催化下发生自由基仿生氧化偶联反应,合成得苯并二氢呋喃环结构化合物1,1经甲基化反应得2．1和2分别在无水碳酸钾、10％氢氧化钠水溶液等不同的碱性条件下进行反应,获得了11个苯并二氢呋喃环开环产物,即8—5′新木脂素类化合物3a～9b,实现了由苯并二氢呋喃新木脂素向8—5′新木脂素的转变,也为合成芪类化合物提供了一种新方法．C-8位上的吸电子基团如酯基的影响使苯并二氢呋喃环易在碱性条件下开环形成8-5′新木脂素类化合物．所合成化合物的结构由MS,IR,^1H NMR和^13C NMR进行了表征．     

Efficient and mild one-pot synthesis of (E)-8′-arylidene-5′,6′,7′,8′-tetrahydrospiro[oxindole-3,4′-pyrano[3,2-c]pyridin] derivatives with potential antitumor activity

A mild and efficient cyclization procedure for the synthesis of (E)-8′-arylidene-5′,6′,7′,8′-tetrahydrospiro[oxindole-3,4′-pyrano[3,2-c]pyridin] derivatives was achieved via one-pot three-component condensation of isatins, malononitrile and (E)-3-arylidene-1-methylpiperidin-4-ones using piperidine as an efficient catalyst and ethanol as an environmentally benign solvent. The in vitro antitumor activity of these compounds was evaluated in human cervical carcinoma cell line (Hela), human liver hepatocellular carcinoma cell line (HepG2), and human breast carcinoma cell line (MDA-MB-231).     

6,6′-Dibromo-3,3′-dimethoxy-2,2′-dihydroxy-1,1′-biphenyl: preparation and resolution

A pratical route to prepare the title biphenyl 1 starting from 3,3′,2,2′-tetramethoxy-1,1′-biphenyl 2 is described. Resolution of 1 was achieved by its conversion into the corresponding diastereomeric menthyldicarbonate. The absolute configuration of (P)-(+)-1 was confirmed by X-ray analysis of the related diastereomer.     

Synthesis of 1′-substituted 4′,4′-dimethyl-6′-methoxy-4′H-spiro[cyclohexane-1,3′-isoquinolines]

The reaction of 1-(4-methoxyphenyl)-1-(1-methylcyclohexyl)ethanol with nitriles in concentrated sulfuric acid afforded 1′-substituted 6′-methoxy-4′,4′-dimethyl-4′H-spiro[cyclohexane-1,3′-isoquinolines] as a result of consecutive Wagner-Meerwein rearrangement and Ritter reaction.     

一个8-O-4′新木脂素化合物的对映选择性合成

报道了一条立体选择性合成赤式8-O-4′新木脂索的新路线，以Sharpless双羟化反应构筑2个手性中心，经过几步转化，得到关键中间体6，通过Mitsunobu反应进行偶联，可以得到单一赤式的8-O-4′新木脂索化合物．通过此路线，立体选择性地合成了一个天然8-O-4′新木脂素的赤式异构体。     

新试剂2-(8′-羟基喹啉-5′-磺酸-7′-偶氮)-变色酸二阶导数光度法测定微量镁

以新试剂2-(8′-羟基喹啉-5′-磺酸-7′-偶氮)-变色酸(简称8Q5SAC)作为显色剂,在硼砂-氢氧化钠缓冲体系中,用二阶导数吸光光度法测定微量镁。镁在0～15/μg/25ml中符合比耳定律,可不经分离直接测定水样中镁,结果满意。