Synthesis and polymerization of 1-(2-N-aziridinoethyl)-4-vinylbenzene

An addition reaction of aziridine onto 1,4-divinylbenzene (DVB) catalyzed by lithium aziridide was studied. It was found that 1-(2-N-aziridinoethyl)-4-vinylbenzene (AEVB) and 1,4-bis (2-N-aziridinoethyl)-benzene(BAEB) can be prepared selectively under appropriate conditions. On the basis of kinetic studies, the reactivity of aziridine toward DVB was compared with that of diethylamine. Vinyl polymerization and ringopening polymerization of AEVB were also carried out to obtain poly [1-{4-(2-aziridinoethyl)phenyl}ethylene] (poly(AEPE)) and poly[{(4-vinylphenethyl) imino}-ethylene](poly(VPIE)), respectively.     

The synthesis and characterization of new polymerizable pyrimidines: Immobilization of the monomers onto hydrophilic graft copolymeric supports through radiation-induced copolymerization–grafting

Polymerizable quaternary allyl-pyrimidinium salts, that is, 1-allyl-4- amino-5-phenyl-pyrimidine (IV), 1-allyl-4-acetamido-5-phenyl-pyrimidine (V), 1-allyl-5-hydroxymethylamino-5-phenyl-pyrimidine (VI), and 1-allyl-pyrimidine (VIII) bromides, as well as 4-acrylamido-5-phenyl-pyrimidines II` and IV`, were synthesized and characterized. Three of the activated pyrimidine derivatives, the two acrylamido and one allyl pyrimidine, were immobilized onto (Agar-g-co-HEMA)-X-TMPTA via graft copolymerization. Each copolymer system, based on 2-hydroxyethyl methacrylate (HEMA) grafted onto Agar followed by crosslinking with trimethyllopropane triacrylate (TMPTA), was prepared by radiation-induced copolymerization carried out in the simultaneous mode. The release properties of the immobilized pyrimidines were assessed in various aqueous media over a period of approximately 22 days. © 1998 John Wiley & Sons, Inc. J. Appl. Polym. Sci. 70: 211–218, 1998     

十二胺基葡萄糖醇盐酸盐的合成

介绍了十二胺基葡萄糖醇盐酸盐的合成方法,并通过正交实验讨论了反应物用量比、反应时间、反应温度对产率的影响,另外改进了目标产物的分离提纯手段,简化了操作,降低了成本。     

Synthesis and polymerization of 2-(β-N-ethylenediphenylamine)-2-oxazoline

Summary The synthesis of 2-(-N-ethylenediphenylamine)-2-oxazoline and its living cationic polymerization in the presence of methyltosylate are described. This 2-substituted 2-oxazoline was used for the synthesis of a ABA triblock copolymer with poly(N--(N-diphenylamine)propionylethylenimine) as A block and poly(ethyleneglycoladipate) as B block.     

Synthesis and polymerization of 2-(β-N-3′-halogencarbazolylethyl)-2-oxazolines

Summary The synthesis of three novel oxazoline monomers,all of which contain 3-halogen substituted carbazolyl groups [i.e., 2-(-N-3 chlorocarbazolylethyl)-2-oxazoline, 2-(-N-3 bromocarbazolylethyl)-2-oxazoline and 2-(-N-3 iodocarbazolylethyl)-2-oxazoline]and their polymerization is described.     

Unusual polymerization of 3-(trimethoxysilyl)-propyldimethyloctadecyl ammonium chloride on PET substrates

3-(Trimethoxysilyl)-propyldimethyloctadecyl ammonium chloride (AEM 5700) is a trifunctional monomer that can be polymerized under acidic conditions at temperatures greater than 100 °C. Under such conditions, coatings based on AEM 5700 formed on PET substrates are relatively hydrophobic and exhibit rewetting times higher than 100 min. Hydrophilic coatings exhibiting a rewetting time of 2.8 min can be also formed when AEM 5700 is initially hydrolyzed under alkaline conditions and then polymerized under acidic conditions. This effect could be related to the accessibility of unreacted hydroxyl groups and quaternary ammonium groups for interaction with water. Excellent antimicrobial action was demonstrated for all coatings based on AEM 5700 on PET substrates. Polyester fabrics having AEM 5700 coating can be dyed with direct dyes. The loss of hydrophilic properties for AEM 5700 coatings is observed after dyeing with direct dyes.     

2-(2-氯苄基)-2-(1-氯环丙基)环氧乙烷的合成

报道了丙硫菌唑中间体2-(2-氯苄基)-2-(1-氯环丙基)环氧乙烷的合成方法。以1-氯-N,N-二甲基环丙基甲酰胺和邻氯氯苄为原料,经格氏反应制备2-氯苄基-(1-氯环丙基)酮;后者再与硫叶立德试剂反应得到相应的环氧化物。     

Synthesis and Surface Properties of Novel Carboxylic Ester-Containing Imidazolium-Based Zwitterionic Surfactants: Monoalkyl 2-(3-Methylimidazolium-1-yl) Succinate Inner Salts

A series of carboxylic ester‐containing imidazolium‐based zwitterionic surfactants, namely, monoalkyl 2‐(3‐methylimidazolium‐1‐yl) succinate inner salts (C_nMimSU, n = 8, 10, 12 and 14), have been synthesized. Their structures were confirmed by ¹H NMR, ¹³C NMR and FTIR. The typical physicochemical properties parameters such as isoelectric point, critical micelle concentration (CMC), surface tension at CMC (γ_CMC), surface pressure at CMC (Π_CMC), adsorption efficiency (pC₂₀), the maximum surface excess (Γ_m), the minimum molecular cross‐sectional area (A_min) and the value of CMC/C₂₀ were determined. The effect of the long‐chain length on the important physicochemical properties of C_nMimSU was studied. It is found that the surface activity of C_nMimSU is enhanced with the long‐chain length increases.     

1—（2—溴苯基）—2—丙醇的合成

以邻溴苯甲醛及硝基乙烷为原料,合成了１－（２－溴苯基）－２硝基丙烯,经氧化得邻溴苯基因酮,再用四氢化铝锂还原合成了标题化合物。经外红、质谱、核磁共振分析确定 了化合物的结构。     

1-羟乙基-2-苯并咪唑氨基甲酸甲酯和1-乙基(2’一丙烯酸酯-1’-基)-2-苯并咪唑氨基甲酸甲酯的合成及用薄层一紫外分光光度法测定其含量

１－乙基（２’－丙烯酸酯－１’－基）－２－苯并咪唑氨基甲酸甲酯是合成多菌灵高 分子化学型缓释剂的重要单体。本文报道了１－乙基（２’－丙烯酸酯－１’－基）－２－苯并 咪唑氨基甲酸甲酯及其制备过程中的中间体－１－羟乙基－２－苯并咪唑氨基甲酸甲酯的 合成和分析方法。     

1-(2-氯苯基)-2-(4-氟苯基)-3-溴-1-丙烯的合成

1-(2-氯苯基)-2-(4-氟苯基)-3-溴-1-丙烯(2)是氟环唑的关键中间体。以1,2-二氯乙烷和水为溶剂,1-(2-氯苯基)-2-(4-氟苯基)-1-丙烯(1)在氢溴酸/双氧水体系中发生α-溴代反应得到该化合物。通过使用氢溴酸/双氧水代替溴素或N-溴代丁二酰亚胺,提高了溴的利用率及产品的收率,避免了烯烃的加成,减少了副反应的发生,减少了三废。通过实验获得了反应的优惠条件:二氯乙烷和水为溶剂,回流反应,n(1)∶n(HBr)∶n(H2O2)=1∶1.1∶2.5,氢溴酸和双氧水的滴加时间为6 h,在上述反应条件下,反应收率为90.6%,选择性90.6%。     

Synthesis and characterisation of novel methyl methacrylate-2-(dimethylamino)ethyl methacrylate copolymer salts containing polymerisable anions

A series of copolymers containing different ratios of methyl methacrylate and 2-(dimethylamino)ethyl methacrylate has been synthesised by conventional free radical polymerisation. These copolymers have been converted into a series of novel salts by reaction with the acid monomers, methacrylic acid, methacryloyloxyethyl phosphate and vinyl phosphonic acid. The copolymers and the corresponding salts have been characterised fully by a range of spectroscopic and thermal analysis techniques. The nature of the salt has a characteristic effect on the thermal degradation of the polymer. The presence of the phosphorus monomers leads to formation of residual char, even at temperatures as high as 1000 °C.     

(S)-1-(2-氯乙酰基)吡咯烷-2-甲腈的合成与表征

探讨了合成(S)-1-(2-氯乙酰基)吡咯烷-2-甲腈的新工艺路线,即以L-脯氨酸为原料,经N-氯乙酰化、羧基氨基化和酰胺脱水反应合成目标化合物。目标化合物及各中间体的结构采用1HNMR和MS进行了确定。此外,详细研究了反应条件的影响,得到了优化的反应条件。目标产物的总收率可达42.3%。该合成路线具有原料便宜易得、操作简单、条件温和等优点,具有很好的市场应用前景。     

Synthesis and characterization of trichlorotitanium 2-(2-pyridinyliminomethyl)phenolates and their ethylene (co-)polymerization behavior

The series of trichlorotitanium 2-(2-pyridinyliminomethyl)phenolates, [4,6-tBu₂C₆H₂O-2-CHNC₅R^1-4N]TiCl₃ (R^1-4 = H (1); R^1,3,4 = H, R² = Me (2); R^1,2,4 = H, R³ = Me (3); R^2,4 = H, R^1,3 = Me (4); R^1,3 = H, R² = CF₃, R⁴ = Cl (5)), were synthesized and characterized by elemental analysis and ¹H/¹³C NMR spectroscopy. The molecular structures of the representative complexes 2 and 4 were confirmed by single-crystal X-ray diffraction, and revealed distorted octahedral geometry at titanium. In the presence of MAO, all titanium pro-catalysts showed good activities for ethylene polymerization with good thermal stability at the optimum temperature of 50 °C. In comparison with the ethylene polymerization results, the activity observed for the co-polymerization of ethylene/1-hexene was far lower, but the polymers produced were of high molecular weight. For the co-polymerization of ethylene/1-octene, enhanced catalytic activity was observed, with 1-octene incorporation of up to 3.83 mol%.     

Synthesis and degradation of nucleic Acid components by formamide and cosmic dust analogues

We show the unprecedented one-pot synthesis of a large suite of pyrimidines (including cytosine and uracil) and purines from formamide in the presence of cosmic-dust analogues (CDAs) of olivines. Since the major problem in the origin of informational macromolecules is the instability of their precursors, we also investigate the stabilizing effect of CDAs on the intrinsic instability of oligonucleotides in formamide.     

(S)-4-(甲硫基)-2-[2-羰基-1-吡咯烷基]丁酰胺的合成

(S) 2 氨基 4 (甲硫基)丁酸甲酯盐酸盐于浓氨水中,发生酰胺化反应,制得(S) 2 氨基 4 (甲硫基)丁酰胺,收率63%;(S) 2 氨基 4 (甲硫基)丁酰胺用甲醇溶解,与浓盐酸成盐,得(S) 2 氨基 4 (甲硫基)丁酰胺盐酸盐,收率66%;(S) 2 氨基 4 (甲硫基)丁酰胺盐酸盐在相转移催化剂四丁基溴化铵(TBAB)及研细氢氧化钾的作用下,与4 氯丁酰氯发生取代、环化反应,制得(S) 4 (甲硫基) 2 [2 羰基 1 吡咯烷基]丁酰胺,收率61%。产品的结构经TLC、IR、1HNMR等进行了表征。     

2-[1-[1'-溴)-乙基]-2-(6'-甲氧基-2'-萘基)-1,3-二氧戊环的合成

以2-溴-1-(6'-甲氧基-2'-萘基)丙-1-酮为原料,乙二醇为缩酮化反应试剂,通过对溶剂和催化剂以及合成工艺参数等研究,得到了合成2-[1-(1'-溴)-乙基]-2-(6'-甲氧基-2'-萘基)-1,3-二氧戊环的优化工艺条件.研究结果表明,在优化的工艺条件下,产物的收率达到了85%.     

4-硝基苯基-2'-溴乙醚的合成

4-硝基苯基-2＇-演乙醚是甲烷磺酰胺苯乙胺类抗心率失常药多非利特（Dclfetilide）的中间体。该化合物以对硝基苯酚和1,2-二滇乙烷为原料经Williamson反应而成,本文对该反应的溶剂、温度、时间、配比等条件和抑制副反应的方法进行了探讨,得到了收率高、质量好、操作简单、三废较少的适合工业化的工艺条件。     

1-(2-羟基苯基)哌嗪氢溴酸盐的合成

1 - (2 -甲氧基苯基 )哌嗪氢溴酸盐是苯基哌嗪类抗高血压药物的一个重要中间体。以 1 (2 -甲氧基苯基 )哌嗪氢溴酸盐为原料 ,经 48%氢溴酸与醋酐 (1∶1)脱甲基得 1- (2 -羟基苯基 )哌嗪氢溴酸盐 ,将所得产物用红外光谱测定其结构 ,结果证实合成样品的结构与目标化合物一致。