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The reaction of polyfluoroalkyl iodides with 4-pentenoic acids in the presence of sodium dithionite at room temperature in aqueous acetonitrile solution [CH〓CN: H〓O=3: 1 ] to gave the corresponding adducts, the latter could form γ-lactones 31~51 in the same medium in 62~92% yield.

室温下,在乙腈/水[3:1]的介质中,多氟烷基碘化物在连二亚硫酸钠的存在下与4-戊烯酸及其在2或3位上具有取代基团的衍生物进行反应,反应2~5h,起先生成两者的加成物,该加成物无需分离,在同一介质中,可进一步反应得到相应的多氟烷基取代的γ-丁内酯31~51,产率62%~92%。

The influence of each condition on the reaction speed and yield was studied, and the optimal conditions were: the ratio of the amount of substance of aromatic amine and heptafluoro-isopropyl iodine was 1:1.1~1.5, the amount of substance of sodium dithionite, sodium bicarbonate, aniline compounds were respectively 1.1~1.3, the amount of substance of phase transfer catalyst TBAB and aniline compounds was 0.05~0.1, the concentration of aniline compound was 0.5~1.0 mol/L, reaction temperature was 10~20 ℃, and the solvent was aether.

最佳结果为:芳胺与七氟异丙基碘的物质的量比1:1.1~1.5,连二亚硫酸钠、碳酸氢钠与苯胺的物质的量分别为1.1~1.3,相转移催化剂四丁基溴化铵与苯胺的物质的量比在0.05~0.1,溶剂总用量使苯胺浓度在0.5~1.0 mol/L;反应温度10~20℃;溶剂采用乙醚。取代基供电子性越强,反应时间越短,产率越高;氨基的对位优先反应,氨基的邻位较难发生反应;且七氟异丙基总是优先取代在芳环电子云密度较高的位置上。

In addition, ioding was found to be an efficient catalyst for the imino Diels-Alder reaction of N-arylimine and enol ethers and the reaction provided tertrahydroqinolines in good yields. One pot synthesis of tetrahydroqinolines from aldehyde, aniline and enol ethers was also achieved using iodine as the catalyst. The chemical yield of the"one pot"reaction was comparable with that obtained using preformed N-arylimine.

此外我们也发现碘能够有效地催化N-芳基亚胺与烯醇醚的Diels-Alder反应,以很高的化学收率得到了四氢喹啉衍生物,并且发现碘也能够直接催化芳香醛、苯胺、烯醇醚的三组分"一锅"反应,获得的化学产率与使用预制的N-芳基亚胺相当。

After more than 20 years I-supplement, typical congenital myxedema has almost been controled in our country.

在政府二十多年的全民补碘后,碘缺乏所致的典型的克汀病已基本得到控制,但是仍有许多亚临床克汀病弱智儿童出现,故认为硒可能是亚克汀病的一个重要的碘外因素。

In part one, the reactions of some active fluorine-containing compounds such as 2, 2-dihydropolyfluoroalkanoic acids and ethyl 2-hydropolyfluoroalkenoates were studied and various fluorine-containing heterocyclic compounds were synthesized. Using 2, 2-dihydropolyfluoroalkanoic acids as the starting material, 4-fluoroalkyl quinolin-2-ols, 2- [ -1-hydropolyfluoro-1-alkenyl] -4H-3, 1-benzoxazin-4-ones, 1-aryl -4, 9-dihydro-3-fluoro-alkyl-1H-pyrazo [3, 4-b] quinolin-4-ones, 5-fluoroalkyl-12H-quin olino [2, 1-b] quinazolin-12-ones, 4-fluoroalkyl-1, 3-dihydro-1, 5-benzodiazepin-2-ones and 4-fluoroalkyl-2H-pyrido [1, 2-a] pyrimidin-2-ones were synthesized through its condensation reaction with anilines, anthranilic acid, N'-aryl-o-aminobenzamides, o-nitro aniline, o-amino pyridine and their derivatives and the subsequent transformations. 5-Fluoroalkyl isoxazolidines, 3-fluoro-3-fluoroalkylisoxazolidino [4, 3-c] quinolin-4-ones, 3-fluoroalkylisoxazolino [4, 3-c] quinolin-4-ones and 2-aryl-3per fluoroacylindoles were synthesized by inter-and intramolecular 1, 3-dipolar cycloaddition of fluorine-containing olefins and nitrones.

第二部分,我们研究了α,α-二氟苄基卤类化合物的亚磺化脱卤反应、产物的转化及全氟烷基亚磺酸盐与芳环化合物的全氟烷基化反应,发现全氟苄基碘或溴及α,α一二氟苄基溴在保险粉等亚磺化脱卤试剂引发下可生成相应的亚磺酸盐;全氟苄基亚磺酸盐与氯气或溴反应可生成全氟苄基磺酰氯或磺酰溴;在烯烃存在下,全氟苄基碘则与烯烃发生加成反应,生成相应的1:1加成产物;在三价醋酸锰的作用下,部分芳香化合物如茴香醚,二甲氧基苯,吡啶,喹啉等可以和过量的全氟烷基亚磺酸盐发生双全氟烷基化反应,反应表现出一定的区域选择性,产率良好。

The major contents in this thesis are described as follows:(1) Seven new thiol fluorescence reagents containing 2-phenylbenzoxazole (or 2-phenylbenzothiazole) derivatives or benzanthrone as fluorphore and iodinacetylamine or maleimide as reaction groups have been synthesized.

本论文的研究工作主要分为以下几个方面:(1)以碘乙酰胺或马来酰亚胺为反应基团和以2-芳基苯并噁唑类化合物或苯并蒽酮为荧光团,首次合成了七种新的碘乙酰胺类和马来酰亚胺类巯基荧光试剂。

In addition, ioding was found to be an efficient catalyst for the imino Diels-Alder reaction of N-arylimine and enol ethers and the reaction provided tertrahydroqinolines in good yields. One pot synthesis of tetrahydroqinolines from aldehyde, aniline and enol ethers was also achieved using iodine as the catalyst. The chemical yield of the"one pot"reaction was comparable with that obtained using preformed N-arylimine.

此外我们也发现碘能够有效地催化N-芳基亚胺与烯醇醚的Diels-Alder反应,以很高的化学收率得到了四氢喹啉衍生物,并且发现碘也能够直接催化芳香醛、苯胺、烯醇醚的三组分&一锅&反应,获得的化学产率与使用预制的N-芳基亚胺相当。

Analysis on main points for determination of chlorine dioxide by iodometric method ;2. The experiment results show: To measure sulfide in wastewater by iodometric method may have errors because the interferent can not be removed.

用碘量法测定废水中的硫化物,可能因无法消除干扰而使测定结果存在较大误差;对于同一废水样品,当碘量法和亚甲基蓝分光光度法的测定结果存在显著性差异时,可用Pb2半定量法进行判定;对于某些化纤企业的废水,用氢氧化钾-乙醇溶液洗涤沉淀,可消除碘量法测定的干扰。

We studied reactions of sulphoxide with aliphatic and aromatic 1,3-dicarbonyl compounds promoted by Cu2·H2O, 2,2′-biimidazole and iodobenzene diacetate, with the presence of K2CO3 as a base and DMSO a solvent.

我们以K2CO3作为碱,DMSO作为反应的溶剂,在二醋酸碘苯、Cu2·H2O、2,2′-联咪唑体系中,对脂肪族和芳香族的1,3-二羰基化合物和亚砜的反应进行了研究。

The electronic effect of para substituents and both the steric and electronic effect of meta substituents in the substituted iodosobenzene were well linear correlated to the yields of cyclohexanol.

取代亚碘酰苯中对位取代基的电子效应和间位取代基的电子及立体效应对氧化产物环己醇的产率有良好线性相关性。

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