荧光法测定铍的研究

研究了新荧光试剂 7 [(2 ,4 二羟基 5 羧基苯 )偶氮 ] 8 羟基喹啉 5 磺酸 (DHCPAQS)与铍络合的反应条件及测定方法。在pH 8.0硼砂体系的缓冲介质中形成R∶Be =2∶1型的强荧光配合物 ,其λex/λem=362nm/ 497nm。铍含量在 0～ 0 .2 0mg·L- 1范围内呈线性关系 ,检出限为 2 .2×10 - 6 mol·L- 1。该方法应用于合金样中痕量铍的测定 ,结果满意。     

Intercalation of pyridine and quinoline intoα-zirconium phosphate

The uptake of pyridine and quinoline into-zirconium phosphate has been investigated by the batch method. The effect of solvent on the reactions was also studied. Pyridine was taken up from ethanol, chloroform, carbon tetrachloride, ethanol-water, and acetone-water solutions, but not from pure acetone at 25°C. Water accelerated the uptake of pyridine. These facts indicate that a water molecule was involved in the uptake reaction of pyridine.Quinoline was taken up easily in an ethanol-water solution at 25°C, and in an ethanol solution at the boiling point. Two reactions — ion exchange and intercalation — occur on taking up the quinoline. An IR spectrum of the quinoline form is reported.     

The potential use of 6-amino-5-methoxy(methyl)-2,3-dimethyl-and 6-amino-5-methoxy(methyl)-1,2,3-trimethyl-indoles in the synthesis of pyrrolo[2,3-f]quinolines

The reaction of 6-amino-2,3-dimethyl-and 6-amino-1,2,3-trimethyl-5-methoxy(methyl)indoles with 4,4,4-trifluoroacetoacetic ester and of 6-amino-5-methoxy-1,2,3-trimethylindole also with other β-dicarbonyl compounds has been studied. It was found that all of the amines investigated undergo condensation readily to form the corresponding enamines while the possible subsequent cyclization to give pyrrolo[2,3-f]quinolines was found only for the condensation product of 6-amino-2,3,5-trimethylindole with 4,4,4-trifluoroacetoacetic ester. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp 97–103, January, 2006.     

New class of P-stereogenic chiral Brønsted acid catalysts derived from chiral phosphinamides

A new class of NH Brønsted acid organocatalysts that feature P-stereogenic chirality was developed. These catalysts were prepared from P-stereogenic chiral phosphinamides and show similar reactivity to BINOL derived phosphoric acid toward the reduction of quinolines via transfer hydrogenation. It shows that stereoselectivity is induced by the P-chiral environment that is created by the substituents attached to the phosphorous atom, which can be readily tuned and modified.     

新型三环系稠杂环［1,2,4］-三唑并［1,5-a］［1］-苯并氮杂及［1,2,4］-三唑并［1,5-a］-喹啉的合成

α-四氢萘酮的乙氧羰基腙(1)经LTA氧化, 得到α-偶氮-α-乙酰氧基化合物2. 在AlCl3作用下, 化合物2脱去乙酰氧基产生重氮正离子中间体3, 再经与腈的1,3-偶极环加成、 ［1,2］-迁移扩环、 碱性水解和与苦味酸作用, 得到新型［1,2,4］-三唑并［1,5 a］［1］苯并氮杂苦味酸盐6a~6c. 以2,3-二氢-1-茚酮为底物, 采用相同的合成路线, 合成了1,2,4-三唑并［1,5-a］-二氢喹啉苦味酸盐12a~12c.     

用8－氨基喹啉高选择性分光光度法测定痕量锇的研究

研究了用８－氨基喹啉在ｐＨ３．６２的ＨＡｃ－ＮａＡｃ缓冲溶液中测定痕量Ｏｓ（Ⅳ）的分光光度法。常见的非贵金属和贵金属离子不干扰测定，并且选择性较好。Ｏｓ（Ⅳ）与８－氨基喹啉的组成比为１：３，表观摩尔吸光系数ε_（６００）＝１．３×１０~５Ｌ／ｍｏｌ·ｃｍ。在０～１０μｇ／１０ｍＬ范围内符合比耳定律。合成样品分析结果良好。     

气相色谱-质谱法测定纺织品中喹啉及其同分异构体异喹啉的残留量

称取剪碎的纺织品样品1.000g,用甲苯10.0mL于常温下超声提取60min,用注射器移取部分提取液,经0.45μm聚四氯乙烯滤膜过滤,取滤液按仪器工作条件进行气相色谱-质谱法分析。以DB-5MS色谱柱(30 m×0.25 mm,0.25μm)为分离柱,在80~200℃之间以12℃·min^-1的升温速率进行色谱分离。在此条件下可使喹啉与异喹啉完全分离。质谱测定中,采用电子轰击离子源(EI)和全扫描模式定性和选择离子扫描模式定量。上述2种化合物均在10.0~250.0μg·L^-1内与其对应峰面积呈线性关系,其检出限均为0.1mg·kg^-1。以空白样品为基体,在3个浓度水平上加入标准溶液进行回收试验,测得喹啉的回收率为82.9%~92.0%,异喹啉的回收率为85.5%~98.1%,2种化合物测定值的平均相对标准偏差(n=6)依次为2.5%,3.1%。应用所提出的方法分析了纺织品实际样品22个,其中有5个试样检出有此2种化合物存在,其质量分数为1.2~27.8mg·kg^-1,均低于OEKO-TEX■STANDARD 100,2019中的规定限量(50mg·kg^-1)。     

Flow injection method for the fluorimetric determination of Zn with 8-(benzenesulphonamido) quinoline

The development of a fluorimetric method for the determination of zinc, based on the fluorescence of the zinc-8-(benzenesulphonamido) quinoline chelate in a micellar medium of sodium dodecylsulfate, is reported. The detection limit is 0.2 g l^–1, the working range is 0.5–700 g l^–1, and the sample throughput is 145 h^–1. The method was evaluated for the determination of zinc in food samples.A batch procedure for the simultaneous determination of zinc and cadmium, based on the synchronous and derivative spectra, is also proposed.     

烷基膦酸类萃取剂与喹啉类萃取剂N_(601)协萃锗(Ⅳ)的研究

研究了盐析剂浓度和水相ｐＨ值对分配比Ｄ的影响。研究了烷基膦酸萃取剂Ｐ５０７和喹啉类萃取剂Ｎ６０１协萃锗的机理，并对萃取平衡常数和热效应进行了估算。     

Synthetic studies on bradykinin antagonist martinellines: construction of a pyrrolo[3,2-c]quinoline skeleton using silicon-tether RCM reaction and allylic amination

The pyrrolo[3,2-c]quinoline consisting of a core structure of martinellines, the first naturally occurring heterocycle, was prepared through silicon-tether ring-closing metathesis reaction and intramolecular allylic amination as key steps.