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Then Doripenem came into the market in the July ,2005. We studied the synthesis of Doripemen.Firstly, we synthesized the chemical 2 from the starting material------o-hydroxylphenylacylamine through Reformastky reaction, alkylation, Diekmann reaction, enolization, esterification and etc. Secondly, we synthesized the chemical 3 from L — hydroxylproline through the protection of carboxyl, amidogen and hydroxyl group, reduction by NaBr, SN_2 substitution and Mitsumobu reaction.
我们以水杨酰胺为起始原料，经Reformatsky反应、烷基化、Diekmann环合、烯醇化、酯化等反应合成双环母核2；再从L-羟基脯氨酸出发，经酯化保护羧基、保护氨基、保护羟基、硼氢化还原酯得醇、Sn2取代和Mitsumobu反应等合成巯基侧链3；最后由化合物3经脱保护、水解得硫醇，和化合物2在二异丙基乙基胺的作用下缩合，最后Pd／C催化脱保护，历经16步反应最终得到产物多尼培南。
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Generally speaking, the reaction types involvingα-oxoketene--acetals mainly include the regioselective addition-aromatization with organometallic reagents, conjugate addition-cyclization with nitrogen nucleophilicspecies, nucleophilic reactions ofα-carbon, acting as odorless dithiol equivalentsin thioacetalization, Michael additions and [5+1] annulation, as well as the synthetic applications based on the above reactions.
一般来说，基于α-羰基二硫缩烯酮化学的反应主要为：与金属有机试剂的选择性加成反应，与氮亲核体的共轭加成反应，α-碳原子的亲核性及相关反应，烷硫基作为硫醇的替代试剂的应用，α-羰基二硫缩烯酮在碳环、杂环化合物合成中的应用等。
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In this paper, a series of 4,5-dithiacrown ether annulated 1,3-dithiole-2-thiones 8a~8d were prepared via condensing 4,5-bis-1,3-dithiole-2-thione (7) with 1,ω-dimercapto polyglycol derivatives in high dilution. The obvious template effect was found during the synthesis of 8c-8d.
在高度稀释条件下，经4，5-二溴甲基-1，3-二硫杂环戊烯-2-硫酮(7)和多缩乙二醇的1，ω-二巯基衍生物的缩合反应，方便地合成了4，5-位带二硫杂冠醚残基的2-硫代-1，3-二硫杂环戊烯的衍生物8a~8d，中间体硫杂冠醚8c~8d的合成中有明显的&模板效应&。
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In this paper, a series of 4,5-dithiacrown ether annulated 1,3-dithiole-2-thiones 8a~8d were prepared via condensing 4,5-bis-1,3-dithiole-2-thione (7) with 1,ω-dimercapto polyglycol derivatives in high dilution. The obvious template effect was found during the synthesis of 8c-8d.
在高度稀释条件下，经4，5-二溴甲基-1，3-二硫杂环戊烯-2-硫酮(7)和多缩乙二醇的1，ω-二巰基衍生物的缩合反应，方便地合成了4，5-位带二硫杂冠醚残基的2-硫代-1，3-二硫杂环戊烯的衍生物8a~8d，中间体硫杂冠醚8c~8d的合成中有明显的&模板效应&。
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Firstly, 3-ethylthiobutanal was prepared from crotonaldehyde reacting with ethanehiol in triethylamine with high yield. Secondly, methyl acetoacetate was converted to 6-ethylthiohept-3-en-2-one by three steps via hydrolysis, condensation with 3-ethyltio-butanal and dehydration, then 6-ethylthiohept-3-en-2-one was cycloco ndensed with dimethyl malonate by Michael addition and Claisen condensation, followed by saponification and decarboxylation to give the intermediate of 5-(2-ethylthiopropyl)-cyclohexane-1,3-dione.
首先，以巴豆醛与乙硫醇为原料，在三乙胺的催化作用下高收率制得3-乙硫基丁醛；然后从乙酰乙酸甲酯出发，通过碱水解、与3-乙硫基丁醛缩合、脱水三步反应合成6-乙硫基-3-烯-2-庚酮，接着6-乙硫基-3-烯-2-庚酮与丙二酸二甲酯通过Michael加成和Claisen缩合成环，再通过皂化和脱羧反应生成中间体5-[2-丙基]-1，3-环己二酮；再与丙酸酐反应丙酰化，最后与0-3-氯-2-丙烯基羟胺肟化，得到目标化合物烯草酮。
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To synthesize the octreotide, Phe-Leu-Glu-Glu-Leu and C_(15)H_(31)-CO-Lys-Thr -Thr-Lys-Ser peptides, the strategies are as followings: Fmoc- group as protective group for α-NH_2; TBTU, DIEA and HOBt as coupling reagent; and ethanedithiol -phenol - thioanisole - H_2O - TFA ( 2.5:5:5:5:82.5 , V/V ) as cleaving solution.
采用Fmoc固相合成法，以苯并三哗四甲基脲四氟硼酸盐、二异丙基乙胺和1-羟基苯骈三氮唑为缩合剂；苯酚—乙二硫醇—苯甲硫醚—水—三氟乙酸(5：5：2.5：5：82.5，V/V)为切割试剂，合成了奥曲肽、Phe-Leu-Glu-Glu-Leu及C_(15)H_(31)-CO-Lys-Thr-Thr-Lys-Ser三种小分子多肽，并对奥曲肽的合成规模进行了放大。
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The heptanal butyl mercaptal was synthesized with heptanal, sodium thiosuifate and 1bromobutane as raw materials.
以正庚醛、硫代硫酸钠和溴代正丁烷为原料，合成了正庚醛正丁硫醇缩醛。
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Acetaldehyde(0\^1 mol) was treated with n propylthiol(0\^1 mol) at 35 ℃ for 20 min to yiled 72% acetaldehyde propyl mercaptal .
以 0 。1 mol乙缩醛和 0 。1 mol 正丙硫醇为原料，35℃下在四氯化碳中反应，经红外光谱，色谱，质谱，元素分析以及核磁共振谱检测，确证了产物为乙醛正丙硫醇缩醛。
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The beta-thioalkoxyalcohols could be obtained in good yields by the reaction of dialkyl-substituted propargylic dithioacetals with a series of carbonyl compounds.
我们发现在铁触媒和格林那试剂的存在下，利用双烷基取代炔丙基硫缩酮和羰基化合物反应生成的beta-硫烷氧基醇，可以进行不常见的beta-氧消去反应，而得到烯炔衍生物。
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In previous results, Alkyl substituted propargylic dithioacetals treating with butyl lithium then were allowed to react with carbonyl compounds to form homopropargylic alcohol with high yields and highly regioselective.
在本实验室先前的研究中发现，烷基取代炔丙基硫缩酮与正丁基锂进行开环反应后，若是与羰基化合物反应，能够以高产率、具位向选择性的生成高炔丙基醇。
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mercaptan：硫醇<类>
mercaptide 硫醇化合物;硫醇盐 | mercaptan 硫醇 | mercaptalation 缩硫醛作用
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mercapto benzothiazole：巯基苯并噻唑
mercaptan 硫醇 | mercapto benzothiazole 巯基苯并噻唑 | mercaptol 缩硫醇
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mercaptal：缩硫醛
merbromin 汞溴红 | mercaptal 缩硫醛 | mercaptan 硫醇
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mercaptal：醛缩硫醇
-lysin 溶素 | -mercaptal 醛缩硫醇 | -mercaptan 硫醇
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sugar mercaptal：糖缩硫醇
sugar manufacturing machinery 制糖机械 | sugar mercaptal 糖缩硫醇 | sugar metabolism 糖类代谢
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mercaptol：缩硫醇
mercaptoethanol 巯基乙醇 | mercaptol 缩硫醇 | mercaptopurine 巯基嘌呤
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methine：甲碱
-mereaptole 酮缩硫醇 | -methine 甲碱 | -methylene 亚甲基
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thioacetal：醛缩硫醇
-thin 质 | thioacetal 醛缩硫醇 | -thiocarbazone 硫卡巴腙