2,3,4,6-四-O-乙酰基-1-巯基-吡喃葡萄糖的合成

以无水α-D-葡萄糖为原料通过四步反应完成2,3,4,6-四-O-乙酰基-1-巯基-吡喃葡萄糖的合成.首先用α-D-葡萄糖和乙酸酐合成1,2,3,4,6-五-O-乙酰基-β-D-吡喃葡萄糖(Ⅰ),再由(Ⅰ)和溴素、冰醋酸制得2,3,4,6-四-O-乙酰-α-D-溴代吡喃葡萄糖(Ⅱ),然后用(Ⅱ)和硫脲制得2-S-(2,3,4,6-四-O-乙酰基-β-D-吡喃葡萄糖基)-2-异硫脲氢溴酸盐(Ⅲ),最后加入氯仿和偏重亚硫酸钠制得最终产物2,3,4,6-四-O-乙酰基-1-巯基-吡喃葡萄糖(Ⅳ).通过FTIR、元素分析、1HNMR、13C-NMR等手段对产物结构进行了表征.     

N,N,N-三甲基-2-羟基-3-硬脂酰氧基丙基氯化铵的合成与表征

以环氧氯丙烷(ECH)和三甲胺(TMA)为原料,在40 kHz超声辅助下合成了季铵盐型活性醚化剂环氧氯丙基三甲基氯化铵(GTA);GTA在超声辅助下与硬脂酸反应,合成了阳离子单酯表面活性剂N,N,N-三甲基-2-羟基-3-硬脂酰氧基丙基氯化铵(CMESA)。通过元素分析,IR等手段对CMESA进行了表征,并考察了反应温度,n(GTA)∶n(硬脂酸),pH和反应时间等因素对产率的影响。结果表明,CMESA的合适合成条件为:超声频率50 kHz,n(GTA)∶n(硬脂酸)=3∶1,反应温度70℃,反应时间4 h,此条件下CMESA的产率为94.90%。     

Proinflammatory Cytokines (IL-1, -6, -8, -15, -17, -18, -23, TNF-α) Single Nucleotide Polymorphisms in Rheumatoid Arthritis—A Literature Review

Conducted studies highlight that a mixture of genetic and environmental factors is responsible for rheumatoid arthritis (RA) development. This study aimed to analyze the available literature for the relationship between, on the one hand, single-nucleotide polymorphisms (SNPs) in the proinflammatory cytokines genes interleukin-1 (IL-1), -6, -8, -15, -17, -18, and -23, and tumor necrosis factor-alpha (TNF-α), and on the other hand, RA susceptibility, severity, and patients’ response to applied treatment. The PubMed database was searched for sources. Preference was given to articles which were published within the past 20 years. Data indicate that the relationship between selected SNPs in proinflammatory cytokines genes and susceptibility to developing RA is inconclusive, and it depends on the ethnicity of the population. Although the allelic and genotypic frequencies of many SNPs in proinflammatory cytokines genes analyzed did not differ between RA patients and healthy controls, deeper analysis showed that these polymorphisms have a relationship with clinicopathological features of RA. SNPs in proinflammatory cytokines genes also “modify patients’ response” to applied treatment. Further studies, on larger cohorts of subjects and in different populations, should be conducted to elucidate the role of SNPs in IL-1, -6, -8, -15, -17, -18, and -23, and TNF-α genes in RA patients.     

环保型脲醛胶生产消费现状及发展趋势

阐述了环保型脲醛树脂生产、消费现状及发展趋势.     

O,O-二乙基-O-异螺环-4-烯-3-肟硫代磷酸酯的合成

本文研究了以薯蓣皂素（Diosgenin）为原料合成O，O-二乙基-O-异螺环-4-烯-3-肟硫代磷酸酯的工艺，IR、^1HNMR、MS、熔点测定等手段对合成的化合物结构进行表征，分析其理化性质和波谱特征，确定所合成的化合物为目标化合物。     

Hydrogenation ofcis-9,cis-12-,cis-9,trans-12- andtrans-9,trans-12- Octadecadienoates

The products formed by hydrogenation of methylcis-9,trans-12- andtrans-9,trans-12-octadecadienoates with nickel and platinum catalysts have been compared with those from methyl esters of the naturally occurring all-cis linoleate. Hydrogen uptake is slower for thetrans isomers. Much of the monoene consisted of esters with double bonds at the 9 and 12 positions with their original geometric configurations. Monoenoic esters with double bonds at the 10 and 11 positions were predominatelytrans and apparently formed by conjugation before hydrogenation. Nickel produced more isomerization than platinum but less than previously reported for copper. With both catalysts hydrogenation proceeded both directly and through conjugated intermediates, in contrast to copper in which all hydrogenation is believed to follow conjugation. Presented at the AOCS Meeting, Los Angeles, April 1972. ARS, USDA.     

高反式- 1,4-丁二烯-异戊二烯共聚物

综述了国内外合成高反式－1，4－丁二烯－异戊二烯共聚物的配位催化体系，负离子催化体系，醇（钠）烯催化体系及其共聚物的结构与性能，用核磁共振，红外光谱对其进行了表征，并提出了发展建议。     

(S,S)-2,12-, (S,S)-2,13-, and (S,S)-2,14-diacetoxyheptadecanes: sex pheromone components of red cedar cone midge, Mayetiola thujae

We identified, synthesized, and field-tested the sex pheromone of female red cedar cone midge Mayetiola thujae (Hedlin) (Diptera: Cecidomyiidae), a pest insect in red cedar Thuja plicata seed orchards. Coupled gas chromatographic (GC)-electroantennographic detection analyses of pheromone extract revealed three components (A, B, C) that elicited responses from antennae of males, all of which occurred below the detection threshold of the mass spectrometer and thus had to be identified without spectroscopic data. Taking into account (1) their retention indices (RI) on three GC columns (DB-5, DB-23, and DB-210), (2) intercolumn RI differentials, and (3) the molecular structures of known cecidomyiid pheromones, we synthesized seven candidate pheromone components: 2,10-, 2,11-, 2,12-, 2,13-, 2,14-, 2,15- and 2,16-diacetoxyheptadecanes. Of these, 2,12-, 2,13-, and 2,14-diacetoxyheptadecane had RIs on all columns consistent with those of A, B, and C and elicited strong antennal responses when tested at picogram levels. In field experiments with the twelve stereoselectively synthesized stereoisomers, only the SS-stereoisomers of 2,12-, 2,13-, and 2,14-diacetoxyheptadecane attracted male M. thujae. The three-component SS-stereoisomer blend was more attractive than the 12-component blend of all stereoisomers, suggesting that one or several nonnatural stereoisomers are inhibitory. One-, two-, and three-component lures of the SS-stereoisomers were equally effective in attracting male M. thujae, indicating redundancy in the pheromone. Identification of the M. thujae sex pheromone will allow development of pheromone-based monitoring, and possibly control, of M. thujae populations in T. plicata seed orchards.     

Synthesis ofcis 9, 15-, 8, 15-, and 7, 15-octadecadienoic acid

In connection with the study of autoxidation of someiso-linoleic acids, the 9,15-, 8,15-, and 7,15-octadecadienoic acids have been synthesized by partial hydrogenation of the corresponding diynoic acids. These acids were prepared by coupling ω-iodo-3-alkynes with ω-chloro-1-alkynes by means of sodium amide in liquid ammonia to form ω-chlorohexadiynes, followed by condensation of the corresponding iodine compounds with sodium malonic ester. Part of paper presented by G. J. Henning at the AOCS Meeting, Philadelphia, October 1966.     

有机颜料中间体N,N′—双乙酰乙酰基2—甲基—5—氯代—1,4—苯二胺的合成

以对氯甲苯为原料,经硝化,还原Ｎ－酰化,水解,乙酰乙酰化反应,制成有机颜料中间体Ｎ,Ｎ′－双乙酰乙酰基－２－甲基－５－氯代－１,４－苯二胺。对影响反应的诸因素进行了讨论。     

Allylic hydroxy fatty compounds with Δ5-, Δ7-, Δ8-, and Δ10-Unsaturation

Several novel allylic mono- and dihydroxy fatty compounds were synthesized from Δ5, Δ7-, Δ8-, and Δ10-monounsaturated fatty acids with the selenium dioxide/tert-butyl-hydroperoxide. Chainlengths were C₁₉ for Δ7 and Δ10, and C₂₀ for Δ5 and Δ8 compounds. With a full range of Δ5- to Δ11-unsaturated allylic monohydroxy fatty compounds available, position-dependent effects in the¹³C-nuclear magnetic resonance spectra of these compounds are discussed. The olefinic carbon shift differences in monohydroxy compounds, where the OH group is located between the double bond and the terminal methyl group, were plotted as a function of double-bond distance from C₁. This plot is presumably a rational function. During SeO₂-based hydroxylation, lactonization of the hydroxy groups, located between the double-bond and the carboxyl group, also occurs for Δ5 unsaturation.     

4-(2-N,N-二甲氨基-乙基)磺酰基-苯肼的合成

芳香肼4-(2-N，N-二甲氨基-乙基)磺酰基一苯肼是阳离子荧光增白剂CH制备的重要中间体，采用对位酯为原料，经过水解，加胺得到芳香胺，再经重氮化、还原的合成路线得到。还原过程中采用氯化亚锡作为还原剂提高芳香肼的收率(85％)。用熔点、红外、核磁、元素分析对产品结构进行表证。     

3-丙酰氨基-N,N-二乙基苯胺的合成新工艺

报道了以间丙酰氨基苯胺为原料,在水溶液中,用氯乙和乙基化剂合成3－丙酰氨基－N,N-二乙基苯胺的新工艺,同时还研究了酸结合剂种类及用量,氯乙烷用量,反应温度等因素对反应的影响。     

Icosahedron cage occupancy of structure-H hydrate helped by Xe -1,1-, cis -1,2-, trans-1,2-, and cis-1,4-dimethylcyclohexanes

Four mixtures of 1,1-, cis-1,2-, trans-1,2-, and cis-1,4-dimethylcyclohexanes (hereafter abbreviated DMCH) including H₂O and Xe have been investigated in a temperature range over 274.5 K and a pressure range up to 2.7 MPa. The 1,1-DMCH and cis-1,2-DMCH generate the structure-H hydrate in the temperature range up to 295.2 and 280.2 K, respectively. Especially, very large depression of equilibrium pressure has been observed in the structure-H 1,1-DMCH hydrate system. On the other hand, neither trans-1,2-DMCH nor cis-1,4-DMCH generates the structure-H hydrate in the present temperature range. It is an important finding that the cis-1,4-DMCH does not generate the structure-H hydrate in the presence of Xe, while the mixture of cis-1,4-DMCH and methane generates the structure-H hydrate.     

4、5、6、7单氟代吲哚-2-酮的合成工艺综述

氟代吲哚-2-酮多用于现代医药化工业中,可以作为多种药物重要中间体.经过文献查阅,综述了吲哚酮4、5、6、7位置氟取代化合物的合成方法,一共给出12条路线.