討論了含硫大雜環(huán)化合物的合成方法、結(jié)構(gòu)和光譜特征。以α，_-二鹵代烷與堿α，_-烷二硫醇反應(yīng)，合成了含2-6個(gè)硫原子的12-42元大雜環(huán)。通過芳香族1，2-二硫醇或2-巰基酚與脂肪族α-二鹵代衍生物的反應(yīng)，制備了含硫和氧原子的氧雜硫大環(huán)烷烴。硫大環(huán)烷烴的合成包括二甲醚或α，_烷二羧酸二氯化物與α，_烷二胺的反應(yīng)，然后用LiAlh4或B2H6還原大雜環(huán)二胺。以二羧酸二氯化物與α，_-惡烷二胺反應(yīng)，以及氯磺酰-β-內(nèi)酰胺與乙二醇反應(yīng)制備了氧雜氮雜大環(huán)烷，雙（溴甲基）取代芳烴與雙（巰基甲基）苯的反應(yīng)是合成低聚噻環(huán)烷的一般途徑。以2，6-雙（溴甲基）吡啶與α，_-烷烴二硫醇反應(yīng)制備了含硫環(huán)吡啶衍生物。對(duì)于含有一個(gè)、兩個(gè)或多個(gè)噻吩環(huán)的大環(huán)化合物的合成，基于-噻吩烷羧酸氯化物的分子內(nèi)和分子間酰化、2,5-雙（碳烷氧基烷基）噻吩的酰偶姻縮合和-鹵代烷基取代的噻吩β-酮酯的分子內(nèi)烷基化的一些步驟。研究了含二硫化物和多硫化物的大雜環(huán)化合物的合成路線。合成過程中，均三甲苯或1,3-二甲氧基苯與二硫二氯化物或二硫二氯化物硫化，并氧化二硫醇，以1,3,5-三（巰基烷基）苯與三（溴代烷基）-甲烷或L，3,5-三[4-（巰基甲基）苯基]-苯的反應(yīng)為基礎(chǔ)，合成了雙和三丙烯基環(huán)化合物。以1，3，5-三-[4-（溴甲基）苯基]苯為原料，研究了含硅、碲或鐵的含硫大雜環(huán)化合物的合成方法，并用X射線衍射、核磁共振、紅外光譜、紫外光譜等分析結(jié)果，討論了含硫大雜環(huán)化合物的結(jié)構(gòu)及其導(dǎo)電性和磁性。

Synthetic methods for, and structural and spectroscopic characteristics of sulfur-containing macroheterocycles are discussed. The synthesis of oligothiamacrocycloalkanes is based on the reaction of α, ò-dihaloalkanes with alkali α,ò-alkanedithiolates to form 12-42-membered macroheterocycles with 2-6 sulfur atoms in the ring. Oxathiamacrocycloalkanes containing sulfur and oxygen atoms in the ring have been prepared by reaction of aromatic 1,2-dithiols or 2-mercaptophenols with aliphatic α-ò-dihalo derivatives. The synthesis of thiamacrocycloalkanes involves the reaction of dimethyl ethers or α,ò-alkanedicarboxylic acid dichlorides with α,ò-alkanediamines followed by reduction of the macroheterocyclic diamides with LiAlH4 or B2H6. Oxathiaazamacrocycloalkanes have been prepared in a similar way by reaction of dicarboxylic acid dichlorides with α,ò-oxaalkanediamines as well as by reaction of chlorosulfonyl-β-lactams with glycols.A general synthetic route to oligothiacyclophanes is the reaction of bis-(bromomethyl) substituted arenes with bis-(mercaptomethyl)benzenes. Analogously, sulfur-containing cyclopyridinophanes have been prepared by reaction of 2,6-bis(bromomethyl)pyridine with α,ò-alkanedithiols. For the synthesis of macrocyclic compounds containing one, two, or several thiophene rings, some procedures based on intra-and intermolecular acylation of ò-thienylalkanecarboxylic acid chlorides, acyloin condensation of 2,5-bis(carbalkoxyalkyl)thiophenes, and intramolecular alkylation of ò-haloalkyl substituted β-keto esters of the thiophene series have been developed.Synthetic routes to macroheterocycles containing di-and polysulfide groups are discussed. The synthesis involves sulfurization of mesitylene or 1,3-dimethoxybenzene with disulfur dichloride or sulfur dichloride as well as the oxidation of dithiols.The synthesis of bi-and trimacrocyclic compounds is based on the reaction of 1,3,5-tris(mercaptoalkyl)benzenes with tris(bromoalkyl)-methanes or l,3,5-tris[4-(mercaptomethyl)phenyl]-benzene with 1,3,5-tris-[4-(bromomethyl)phenyl] benzene.Some methods for the synthesis of sulfur-containing macroheterocycles containing silicon, tellurium, or iron are considered.The structures of the sulfur-containing macroheterocycles are discussed using the results of X-ray diffraction, H NMR, IR, and UV spectroscopy as well as their electroconductive and magnetic properties.