N,N-二乙基-对二甲氨基苯甲酰胺的合成

以对二甲氨基苯甲酸为原料合成了增感剂N,N-二乙基-对二甲氨基苯甲酰胺,其结构经IR,UV和MS确认.     

N,N-二羟乙基十二烷基胺的合成及性能

以二乙醇胺和溴代十二烷为原料,在无水乙醇介质中合成了脱模剂用新型原材料N,N-二羟乙基十二烷基胺.通过正交试验法对合成工艺进行了优化,研究了各种因素对合成产率的影响,确定了在无水乙醇介质中合成该化合物的最佳工艺条件;表征了合成产物的结构,并测定了其理化性能和表面化学性能.结果表明:在无水乙醇介质中合成N,N-二羟乙基十二烷基胺简单易行,产率为85.37%.合成产物在水溶液中的临界胶束浓度为2.92×10-3mol/L,所对应的液体表面张力为20.875 mN/m.以合成产物为原材料制备的固化薄膜的表面能为14.57 mN/m,小于聚氨酯塑料的表面能29 mN/m,是聚氨酯塑料和弹性体脱模剂的理想原材料.     

N，N-二乙基一对二甲氨基苯甲酰胺的合成

以对二甲氨基苯甲酸为原料合成了增感剂N，N-二乙基-对二甲氨基苯甲酰胺，其结构经IR，UV和MS确认。     

甲基丙烯酸β-(N,N-二乙基氨基)乙酯的制备

甲基丙烯酸β-(N,N-二乙基氨基)乙酯是一种带有碱性含氮基团的单体。它的某些共聚物已被用作合成纤维的助染剂、润滑油的浮游分散剂和航空煤油的抗静电增效剂。这种单体还广泛地应用于制备高级装璜树脂、特种印刷油墨以及彩色感光材料。多年来,在实验室制备或小批量生产中,普遍采用以醇钠作催化剂的酯交换法来制取这一单体。由于酯交换速度很慢、聚合现象严重、胺基酯产率只有40—     

N,N-二甲氨基丙烯酸乙酯的制备

报道了一种以二甲氨基乙醇（DEAE）与丙烯酸丁酯（BA）为原料,钛酯四丁酯（TBT）为催化剂,在负压下反应及蒸馏,生产N,N－二甲氨基丙烯酸乙酯（OMAEA）的方法,并讨论了原料配比、催化剂用量、压力与温度及反应气氛对产物收率的影响,提出了优化的反应条件。     

N,N-二(邻硝基苯氨基乙基)甘氨酸糖酯的合成

在氢氧化钠和四丁基溴化铵存在下,将N,N-二(邻硝基苯氨基乙基)甘氨酸分别与O-乙酰基溴代葡萄糖、O-乙酰基溴代半乳糖、O-乙酰基溴代乳糖和O-乙酰基溴代木糖作用,制得N,N-二取代甘氨酸的对应乙酰基糖酯。由元素分析、IR、MS和¹HNMR确认了4个的糖酯的结构。关键词N,N-二(邻硝基苯氨基乙基)甘氨酸糖酯,溴代葡萄糖,溴代乳糖,溴代木糖,葡萄糖酸酯。     

N,N-二(邻硝基苯氨基乙基)甘氨酸糖酯的合成

在筛选抗植物病毒剂的研究中发现N,N-二(邻硝基苯氨基乙基)甘氨酸具有较好的抑制烟草花叶病毒(TMV)的活性,为提高其抗病毒活性,根据一些糖酯具有生理活性,而且它们的活性和药理性质都比同系物非糖酯要好,因此决定合成标题酸的酯基葡萄糖、乳糖、半乳糖和木糖酯,这些酯均为新化合物。     

伯芳胺的N-吡啶乙基化和N,N-二(吡啶乙基)化反应

在我们另一项工作中需要合成一些在芳胺N上含有两个吡啶N的三齿配体。以2-乙烯吡啶与伯芳胺加成,除与4-甲氰基苯胺产生不纯的N,N-二(吡啶乙基)衍生物外,与所有其它伯芳胺都只产生N-吡啶乙基衍生物,而没有相应的N,N-二(吡啶乙基)衍生物。我们以三氟乙酸为催化剂修饰文献的方法,用过量的2-乙烯吡啶与伯芳胺加成,     

N,N-二烷基酰胺萃取硝酸的性能

酰胺萃取剂的羰基氧具有很强的碱性,易萃取酸.考虑到酰胺萃取酸后对其萃取金属离子的性能有影响,研究酰胺对硝酸的萃取是必要的.     

Synthesis of Carbamoyl-Containing N,S-Heterocyclic Compounds

Monothioxamides unsubstituted at the thioamidic nitrogen atom were obtained by the reaction of NS-morpholino-NO-R-thioxamides with ammonia. Carbamoyl-containing 5-phenylcarbamoyl-1,2,4-dithiazoles, 6-phenylcarbamoyl-5,6-dihydro-[1,2,4,5]-dithiadiazin-3-one, and 5-phenylcarbamoyl-2-oxy-1,3,4-thiadiazole were synthesized by the reaction of monothioxamides or thiohydrazides of oxamic acids with chlorocarbonylsulfenyl chloride.     

Analysis of Phenoxycarboxylic Acids and Other Acidic Compounds in Tap,Ground, Surface and Sewage Water at the Low ng/1 Level

Abstract

Solid-phase extraction with RP-C18 phase has been successfully applied for the determination of more than 30 acidic herbicides and related compounds from environmental water samples. Detection of these contaminants was performed after pentafluorobenzylation at the low ng per liter level using gas chromatography/mass spectrometry. With multiple-component SIM programming simultaneous detection of all compounds in one single gas chromatographic run was possible.

Increased reliability of acidic herbicide analysis from water samples with high matrix content was achieved by using a surrogate as well as an internal standard. 2-(4-chlorophenoxy) butyric acid, being a structural isomer of clofibric acid and mecoprop, was chosen as surrogate standard because cloflbric acid was found to be a widespread contaminant in environmental water samples from the Berlin area. Mecoprop, dichlorprop and 1-naphthylacetic acid were also found in field studies of some of these samples. A few examples of positive findings in tap, ground, surface and sewage water samples are presented.     

负载型杂多酸催化下N2O5对氯苯的选择性硝化

使用负载型杂多酸为催化剂,N2O5为硝化剂的新型硝化体系,对氯苯的硝化反应进行研究. 分别考察了杂多酸类型、载体种类、杂多酸负载量及催化剂循环使用次数等因素对硝化反应的影响. 结果表明,N2O5硝化反应属于酸催化反应,负载型杂多酸能显著提高N2O5的硝化能力;催化剂回收后可直接重复使用,催化活性没有明显的降低. 在优化条件下,氯苯硝化反应得率为26%,对位选择性达68.8%. 结果表明,N2O5是一种具有应用前景的硝化试剂,可取代传统的硝硫混酸硝化法,减少废酸处理,符合绿色环保要求.     

Simple, Rapid, and Sensitive Determination of Odorous Compounds in Water by GC–MS

A gas chromatographic–mass spectrometric method has been developed for rapid and sensitive determination of odorous compounds in water. The water sample (200 mL), at pH 6.5, was extracted with 1 mL pentane in a 250-mL separatory funnel. Fluorobenzene was added to the water sample as internal standard and the solution was mechanically shaken for 5 min and analyzed by GC–MS, with selected ion monitoring, without further concentration or purification steps. The peaks had good chromatographic properties and extraction of the compounds from water resulted in relatively high recoveries with small variations. The detection limits of the assay were 0.1 ng L^–1 for 2-isopropyl-3-methoxypyrazine, 2-isobutyl-3-methoxypyrazine, 2-methylisoborneol, and geosmin, 0.5 ng L^–1 for anisole, and 1.0 ng L^–1 for 2,4,6-trichloroanisole and trans, trans-2,4-heptadienal. Turn-around time was one day for up to approximately 40 samples. The method is simple, convenient, and can be learned easily by relatively inexperienced personnel. It was used to analyze seven odorous compounds in water from Decheung-Lake in Korea, and raw and treated water originating from the same lake. In the summer of 2001 significant levels of anisole (up to 225 ng L^–1) were observed, and geosmin and 2-methylisoborneol were detected at concentrations of up to 23.8 and 26.7 ng L^–1, respectively. 2-Isopropyl-3-methoxypyrazine, 2-isobutyl-3-methoxypyrazine, and trans, trans-2,4-heptadienal levels during that period were not significant. The method can used for simultaneous detection of several odorous compounds in water.     

N, N'-二芳基己二酰双偶氮化合物的合成及其结构表征

以N, N'-二芳基己二酰二肼类化合物为原料,用Fe(NO3)3·9H2O作氧化剂,在室温无溶剂条件下将N, N'-二芳基己二酰二肼类化合物氧化脱氢为N, N'-二芳基己二酰双偶氮化合物.产物结构经元素分析、IR、 1H NMR确证,原料的IR谱中在3200～3400cm-1出现的2个N-H吸收峰在氧化产物中消失,但在1455cm-1附近有-N=N-吸收峰;1H NMR谱中在δ7.3～10.5之间的2个N-H化学位移在氧化产物中也消失;产物的元素分析结果与理论值基本相符.收率80%～94%.