胞嘧啶的合成工艺改进

以氰乙酸乙酯、尿素、原甲酸三乙酯为原料,经缩合、环化和水解反应合成了5-羧基胞嘧啶(6);6经催化脱羧合成了胞嘧啶,总收率65.7%,其结构经1H NMR和ESI-MS确证。     

三苯胺亚胺类化合物的合成

以三苯胺为起始原料,经硝化、还原和胺醛缩合反应合成了4个三苯胺亚胺类化合物,其结构经1H NMR和IR确证。     

新型甲磺酰基喹啉衍生物的合成

以7-羧基喹啉为原料,经硝化、酯化、喹啉环和硝基的还原、磺酰化和烷基化反应合成了7个新型的甲磺酰基喹啉衍生物,其结构经1H NMR和LC-MS表征。     

盐酸奥洛他定的合成

以对羟基苯乙酸和苯酞为原料,经缩合、环合、Wittig反应等合成了抗过敏药盐酸奥洛他定,总收率12.5%,其结构经1H NMR, IR和MS确证.     

功能性二茂铁单、双乙基咪唑的合成

以单、双乙酰基二茂铁为原料,经还原和脱水反应,高效地合成了单、双齿功能性配体--二茂铁乙基咪唑和二茂铁双乙基咪唑,其结构经1H NMR,IR,MS和元素分析表征.     

经腹联合经阴道彩超在评估凶险型前置胎盘合并胎盘植入中的应用价值

本文对经腹联合经阴道彩超在评估凶险型前置胎盘(PPP)合并胎盘植入中的应用价值进行了探讨。选取我院2017年6月~2019年6月PPP患者172例,所有患者均给予经腹彩超、经阴道彩超检查,以产后病理结果为对照,分析经腹彩超、经阴道彩超,以及二者联合,对PPP合并胎盘植入的评估价值。产后病理结果显示,172例PPP患者中,有合并胎盘植入患者120例(69.77%)、无合并胎盘植入患者52例(30.23%)。对PPP合并胎盘植入的敏感度、特异度、准确度进行评估,结果显示,经腹彩超其值分别为76.67%、73.08%、75.58%,经阴道彩超分别为83.33%、80.77%、82.56%,经腹联合经阴道彩超则分别为96.67%、96.15%、96.51%,二者联合明显高于经腹彩超、经阴道彩超,差异有统计学意义(P<0.05)。证实经腹、经阴道彩超是评估PPP合并胎盘植入的有效检查方法,且二者联合的评估价值更高,值得临床推广。     

法西多曲原料药的合成

以胡椒醛和丙二酸酯为原料,经Knoevenagel缩合、常压催化氢化、缩合、加成、酰化5步反应合成了法西多曲,其结构经元素分析、IR和1H NMR表征。总收率72．1％。     

白鲜碱的合成

以苯胺为原料经取代、关环、甲基化、还原、消除反应合成了呋喃喹啉类生物碱白鲜碱,总收率17%,其结构经1H NMR,13C NMR和MS确证.     

氟替卡松丙酸酯的合成

以双氟美松为原料,经氧化、酯化、酰化、醇解和氟甲基化反应制得氟替卡松丙酸酯(1),总收率60.1%。1和中间体的结构经1H NMR,IR和MS表征。     

三元环氨基酸的合成工艺改进

以甘氨酸乙酯盐酸盐为原料,经酰氨化、脱水、成环、水解反应合成了三元环氨基酸,总收率达50.4%。其结构经1HNMR,13CNMR,IR和EI-MS确证。     

STAT3抑制剂（HO-3867）的合成工艺改进

以3,5-二溴-2,2,6,6-四甲基-4-哌啶酮为起始原料,经Favorskii重排和氧化反应的一锅法制得甲基-1-氧基-2,2,5,5-四甲基吡咯烷-3-羧酸甲酯(5a);低温下用四氢铝锂还原5a制得3-羟甲基-1-氧基-2,2,5,5-四甲基吡咯啉(7); 7溴化后与芳胺发生烷基化反应,半连续合成了STAT3抑制剂（HO-3867）,总产率46.3%,其结构经¹H NMR和HR-ESI-MS确证。     

Green synthesis of hydrotalcite from untreated magnesium oxide and aluminum hydroxide

The influence of reaction temperature and time on the hydrothermal dissolution-precipitation synthesis of hydrotalcite was investigated. Untreated MgO, Al(OH)₃ and NaHCO₃ were used. An industrially beneficial, economically favourable, environmentally friendly, zero effluent synthesis procedure was devised based on green chemistry principles, in which the salt-rich effluent typically produced was eliminated by regenerating the sodium bicarbonate in a full recycle process. It was found that the formation of hydromagnesite dominates at low temperatures independent of reaction time. With an increase in reaction time and temperature, hydromagnesite decomposes to form magnesite. At low temperatures, the formation of hydrotalcite is limited by the solubility of the Al(OH)₃. To achieve a hydrotalcite yield of 96%, a reaction temperature of 160°C for 5?h is required. A yield higher than 99% was achieved at 180°C and 5?h reaction time, producing an layered double hydroxide with high crystallinity and homogeneity.     

硫杂蒽酮的合成和表征

为了寻求合成硫杂蒽酮的高效新方法,以2,2′-二硫代二苯甲酸和苯酚为原料,硫酸为溶剂和催化剂,考察了沸石分子筛、Al2O3和P2O5、温度、原料的物质的量之比、反应时间对反应收率的影响,确定了最佳反应条件,推测了可能的反应过程;进而以2,2′-二硫代二苯甲酸和相应的苯衍生物为原料,在H2SO4-P2O5体系中于最佳反应条件下制备了13个硫杂蒽酮类化合物,并利用柱色谱分离以及红外光谱与核磁共振谱对产物进行表征.结果表明,在反应体系中引入P2O5有利于促进反应的完成;最佳反应条件为:温度70℃、2,2′-二硫代二苯甲酸/苯衍生物物质的量之比1∶6、反应时间6h.邻苯二酚与二硫代水杨酸的反应产物——化合物11(a)和11(b)为同分异构体.     

Syntheses and Preliminary Biological Evaluations of the Dibromopyrrole-Containing Marine Natural Products Agesasine A,Agesasine B,Longamide E and Various Congeners

Total syntheses of the title marine natural products have been achieved and so confirming the structures originally assigned to them. Upon subjecting agesasine A and its corresponding ethyl ester to Mitsunobu conditions, a 1,5-cyclodehydration reaction takes place to give 2-oxazolines. In contrast, on subjecting agesasine B to the same Mitsunobu conditions, a simple dehydration reaction occurs to give the corresponding acrylate. A total synthesis of longamide E was achieved by engaging a 1,2-disubstituted pyrrole in a lactam-forming reaction and this was followed by a two-fold and fully regio-controlled bromination reaction. A distinctly different and possibly biomimetic route was used to synthesize, via the open-chain natural product nakamurine B, longamide B and its methyl ester. Preliminary biological evaluations of the title alkaloids and various analogues against a small human cancer cell line panel reveals cytotoxic properties that vary significantly with structure.     

A Bioinspired Synthesis of (±)‐Rubrobramide, (±)‐Flavipucine,and (±)‐Isoflavipucine

A biomimetic synthesis of naturally occurring lactams rubrobramide, flavipucine, and isoflavipucine is described. The key step is a regioselective Darzens reaction between isobutyl glyoxal and an α‐bromo‐β‐ketoamide. The construction of the core tricyclic ring system of rubrobramide was achieved by a cascade reaction in a single step from an α,β‐epoxy‐γ‐lactam. Furthermore, the absolute configuration of naturally occurring (+)‐rubrobramide was determined by vibrational circular dichroism. (±)‐Flavipucine and (±)‐isoflavipucine were synthesized from an epoxyimide, which was prepared by reaction of isobutyl glyoxal with a protected α‐bromo‐β‐ketoamide. Deprotection of the epoxyimide and formation of the pyridone ring gave (±)‐flavipucine, which was converted into (±)‐isoflavipucine by thermal isomerization.     

一种合成端羧基聚乙二醇单甲醚的新方法

以聚乙二醇单甲醚和丙烯腈为原料,在水相中合成了一端为羧基的聚乙二醇单甲醚,其结构经1H NMR和IR确证。讨论了反应时间、反应温度、溶剂和惰性气氛对反应的影响。     

1,4-双(6-苯基-1,2,4,5-四嗪-3-基)苯的合成

以对苯二甲醛为原料,经过单肼化、腙化、氯化和环合氧化四步反应首次合成1,4-双(6-苯基-1,2,4,5-四嗪-3-基)苯,其结构经1H NMR,IR,MS和元素分析表征。     

烯胺酮(酯)类化合物合成研究进展

本文综述了目前国内外烯胺酮(酯)类化合物的主要合成方法。从采用缩合、加成、取代及杂环分解等不同的反应类型,采用路易斯酸、无机酸等不同的催化剂体系,以及采用微波或超声波促进,利用离子液体作为反应介质等几个方面展开讨论。     

金刚烷基甜菜碱型表面活性剂的合成研究

以金刚烷胺和甲酸、甲醛为原料,经过埃斯韦勒一克拉克甲基化反应合成了N,N-二甲基金刚烷叔胺.随后采用N,N-二甲基金刚烷叔胺与氯乙酸钠通过季铵化反应合成N-(1-金刚烷基)-N,N-二甲基甜菜碱两性离子表面活性剂,并通过探讨溶剂-选择、反应温度、反应时间、反应体系pH值、反应物配比对反应产率的影响,得出金刚烷基甜菜碱的...