钌（Ⅱ）－联吡啶－巴比妥酸－Ce（Ⅳ）化学发光体系测定巴比妥酸的研究

利用巴比妥酸对Ｃｅ（Ⅳ）氧化钌（Ⅱ）－联吡啶化学发光反应的增强作用，建立了痕量巴比妥酸的自动脉冲注射化学发光测定法方法的检出限为１０×１０－９ｇ／ｍＬ，线性范围为５０×１０－８－６．２×１０－５ｇ／ｍＬ巴比妥酸的衍生物如巴比妥、苯巴比妥和戊巴比妥对Ｃｅ（Ⅳ）氧化钌（Ⅱ）联吡啶化学发光反应无增强作用据此对合成样中巴比妥酸作选择性检测探讨了巴比妥酸的增强机理     

巴比妥酸—NO2^—2铁（Ⅱ）—CPB显色体系光度测定巴比妥酸的研究

本文对巴比妥酸－ＮＯ＾－２－铁（Ⅱ）－ＣＰＢ显色体系进行了研究,建立了一种测定巴比妥酸的分光光度法,该法巴比妥酸含量在１．０＊１０＾－６－２．０＊１０＾－５ｇ／ｍＬ范围内符合比尔定律。     

硫代巴比妥酸光度法测定香草醛

香草醛在强酸性介质中与硫代巴比妥酸（ＴＢＡ） 反应生成黄绿色的化合物,建立了可见光分光光度法测定香草醛方法。线性范围１×１０－ ６～１５×１０－ ４ｍ ｏｌ／Ｌ,检出限为４４７×１０－ ８ｍ ｏｌ／Ｌ。对冰淇淋、麦片等进行了其中香草醛含量测定,结果满意     

硫代巴妥酸光度法测定香草醛

香草酸在强酸性介与硫代巴比妥酸（ＴＢＡ）反应生成黄绿色的化合物,建立可见光分光光度法香草醛方法。线性范围１×１０＾－６￣１．５×１０＾－４ｍｏｌ／ｌ,检出限为４．４７×１０＾－８ｍｏｌ／Ｌ。对冰淇淋,麦片等进行了其中香草醛含量测定,结果满意。     

硫代巴比妥酸分光光度法测定消毒液中戊二醛

在醋酸介质中，硫代巴比妥酸与戊二醛生成缩合产物，此产物在可见光区有最大吸收，籍此可测定微量戊二醛。线性范围为０．５－１０．０ｍｇ／Ｌ，检出限为０．０１９ｍｇ／Ｌ。方法灵敏度高，体系简单，操作简便，用本方法测定了消毒液中戊二醛的含量，结果满意。     

偶合化学发光法测定血清中亚硝酸盐

采用正交试验法建立了Ｌｕｍｉｎｏｌ－ＮＯ－２－Ｋ４［Ｆｅ（ＣＮ）６］偶合发光体系测定血清ＮＯ－２的方法。本法测定ＮＯ－２的线性范围为９．０×１０－６～１．０×１０－３μｇ／Ｌ,检出限３．５×１０－６μｇ／Ｌ。对１．０×１０－４μｇ／ＬＮＯ－２连续测定１１次的相对标准偏差为２．３％。用于血清中亚硝酸根的测定,结果满意。     

含有吸附络合物溶液的倒数示波计时电位法的应用

Ｐｂ（Ⅱ）在０．２％乙二胺－５×１０＾－３ｍｏｌ·Ｌ＾－１ＨＯｘ－０．３ｍｏｌ·Ｌ＾－１ＫＯＨ溶液中，有良好的全数示波图，其峰电位Ｅｐ＝－１．０５（ｖｓ．ＳＣＥ），峰高与Ｐｂ＾２＋溶度在４．０×１０＾－７～２．０×１０＾－５ｍｏｌ·Ｌ＾－１内成正比，检测下限可达２．０×１０＾－７ｍｏｌ·Ｌ＾－１。本实验采用倒数示波计时电位法对铝合金“Ａ”中铅进行了测定，并直接通过示波图，对络合物的吸附属于性进行了     

L－色氨酸－H_2O_2－ClO~－－CTAB流动注射化学发光反应的研究

本文采用反相流动注射法研究了在阳离子表面活性剂ＣＴＡＢ存在下，Ｌ－色氨酸－Ｈ２Ｏ２－ＣｌＯ－体系的化学发光行为，对影响化学发光强度的诸因素和表面活性剂的增强作用进行了试验和探讨，建立了化学发光测定Ｌ－色氨酸的新方法。线性范围１．０×１０－８～８．０×１０－６ｍｏｌ·Ｌ－１，检测限为４．０×１０－９ｍｏｌ·Ｌ－１（Ｓ／Ｎ＝２）。对合成试样中三种浓度的Ｌ－色氨酸测定的回收率在９７％～１０６％之间，相对标准偏差小于４％。     

流动注射化学发光法测定甲氨蝶呤

研究了甲醛增强高锰酸钾与甲氨蝶呤的化学发光反应，由此建立了一种测定甲氨蝶呤的流动性注射化学发光分析法，方法的检出限为３．４×１０＾－９ｇ／ｍＬ，相对标准偏差为１．１％（２．０×１０＾－６ｇ／ｍＬ甲氨蝶呤，ｎ＝１１）线性范围为１．０×１０＾－８～１．０×１０＾－５ｇ／ｍＬ。该法已用于甲氨蝶呤针剂及片剂中甲氨蝶呤含量的测定。     

无机还原剂与光泽精化学发光反应的研究Ⅲ．钒（Ⅱ）－光泽精体系的化学发光反应

本文采用装有Ｊｏｎｅｓ柱的流动注射系统，研究了钒（Ⅱ）－光泽精体系的化学发光反应。在此基础上建立了痕量钒测定的新方法。方法的检出限３×１０￣（－１０）ｇ·ｍＬ￣（－１）；对于１．０×１０￣（－７）ｇ·ｍＬ￣（－１）钒标准溶液测定的相对标准偏差为２％（ｎ＝１１）；线性范围１．０×１０￣（－９）～９．０×１０￣（－５）ｇ·ｍＬ￣（－１），相关系数大于０．９９８０。该方法已用于水样中痕量钒的测定。对于反应机理，本文也进行了探讨。     

Spectrophotometric Determination of Barbituric Acid

Abstract

Barbituric acid reacts with chloral hydrate in alkaline media, after heating for 1 min. at 100°C to give an orangish yellow colour having maximum absorbance at 450 nm. The reaction is selective for barbituric acid with 0.01 mg/ml as the visual limit of quantitation and provides a basis for a new spectrophotometric determination. The colour reaction obeys Beer's Law from 0.001 to 0.6 mg/ml and the relative standard deviation is 1.1%. The quantitative assessment of tolerable amounts of other drugs is also studied.     

巴比妥酸在药物合成上的应用

本文综述了巴比妥酸在药物合成上的应用与进展。通过巴比妥酸的烃化、卤化、环化、缩合、光解、螯合等反应得到的一些衍生物具有重要的生理活性，可用作镇静剂、麻醉剂、安眠药、抗肿瘤药、抗菌素等。参考文献２６篇。     

Electrochemical Study of Iodide in the Presence of Barbituric Acid: Application to the Catalytic Determination of Barbituric Acid

Electrochemical oxidation of iodide has been studied in the presence of barbituric acid using cyclic voltammetry and controlled-potential coulometry. The results indicate that the barbituric acid participating in the halogenation reaction converts to an iodo derivative of the parent compound. Moreover, the results are indicative of the suitability of iodide as a mediator for the determination of barbituric acid in aqueous solutions. The quasicatalytic peak current is linearly dependent on the barbituric acid concentration. The calibration graph is parabolic, with two linear sections of 6.0 × 10^–5–1.0 × 10^–3and 1.0 × 10^–3–1.0 × 10^–2M. The relative standard deviation for ten determinations of 2.0 × 10^–4M barbituric acid is 2.1%, and the detection limit of the method is 3.97 × 10^–5M.     

One‐pot New Barbituric Acid Derivatives Derived from the Reaction of Barbituric Acids with BrCN and Ketones

Reaction of cyclic β‐dicarbonyl compounds such as pyrimidine‐(1H,3H,5H)‐2,4,6‐trione (BA), 1,3‐dimethyl pyrimidine‐(1H,3H,5H)‐2,4,6‐trione (DMBA) and 2‐thioxo‐pyrimidine‐(1H,3H,5H)‐4,6‐dione (TBA) with cyanogen bromide in acetone and 2‐butanone in the presence of triethylamine afforded a new class of stable heterocyclic spiro[furo[2,3‐d]pyrimidine‐6,5′‐pyrimidine]2,2′,4,4′,6′(3H,3′H,5H)‐pentaones (dimeric forms of barbiturate) at 0 °C and ambient temperature. Structure elucidation was carried out by X‐ray crystallographic, ¹H NMR, ¹³C NMR, two dimensional NMR, FT‐IR spectra, mass spectrometry and elemental analysis. The mechanism of product formation is discussed. The reaction of DMBA with cyanogen bromide in the presence of triethylamine also afforded trimeric form of barbiturate of uracil derivatives in good yield. The reaction of selected acyclic β‐dicarbonyl compounds with cyanogen bromide in the presence of triethylamine in acetone and/or diethyl ether has also been investigated under the same condition. Diethyl malonate and ethyl cyanoacetate brominated and also ethyl acetocetate both brominated and cyanated on active methylene via cyanogen bromide.     

Determination of pK-Values of Some Barbituric Acid Derivatives

Abstract

Practical dissociation constants (μ = 0.1, 25°C) of the following barbituric acids (pK₁, pK₂) were determined spectrophotometrically: 5-pivaloyloxy-5-(1-phenylethyl) - (7.0; 12.1); 5-hydroxy-5-(1-phenyethyl) - (7.8; 12.0); N-methoxymethy 1 -5-phenyl-5-ethyl (7.3₅; -); N-methyl -5-phenyl -5-ethyl - (7.8; -); 5-phenyl-5-ethyl - (7.3₅; 12.3). Structures were attributed to individual ionic forms involved.     

5-芳亚苄基巴比妥酸的固态合成

固相合成;5-芳亚苄基巴比妥酸的固态合成     

Barbituric acid as a substituent at aryl methylium ions

Activation of different benzophenone derivatives with triflic anhydride for electrophilic aromatic substitution of 5-phenylbarbituric acids leads to regioselective formation of the ortho-substituted product. The resulting triphenylmethylium salt can be isolated when the Michlers ketone is used. More electrophilic cations form cyclic enol ethers such as 1-n-butyl-9,9-diaryl-1,9-dihydro-10-oxa-1,3-diazaphenanthrene-2,4-diones. Alternatively, supramolecular complex formation with 2,6-diacetamido pyridine as well as carbenium ion generation have been studied. Although in dilute acid only protonation of one of the carbonyl oxygens occurs, ring opening of the cyclic enol ether toward the carbenium ion is observed in 96% sulfuric acid.     

Barbituric acid in the synthesis of fused 1,7-phenanthroline derivatives

New 7-aryl(hetaryl)-7,8,9,10,11,12-hexahydropyrimido[5,4-b][1,7]phenanthroline-9,11-diones have been synthesized by three-component condensation of barbituric acid with quinolin-5-amine and aromatic or heteroaromatic aldehydes.     

手性方酰胺催化巴比妥酸和硝基烯的不对称Michael加成反应

用手性环己二胺衍生的方酰胺催化1,3-二甲基巴比妥酸和硝基烯的不对称Michael加成反应,合成了一系列新型巴比妥衍生物,其结构经¹H NMR和¹³C NMR表征。并考察了底物结构对反应收率和立体选择性的影响。结果表明：该反应可获得较高的收率(80%~100%)和中等至良好的对映选择性(ee 43%~90%)。     

Barbituric and thiobarbituric acids: a conformational and spectroscopic study

A conformational study on Barbituric (BA) and Thiobarbituric (TBA) acids was performed at ab initio MP2/6-31G** level on the neutral, protonated, mono- and di-anionic forms. Acid-base equilibria were studied by comparing the electronic transitions evaluated for the most stable conformations and the experimental spectra at different pH values. The electronic transitions were obtained through the ZINDO approach.