新型2－乙内酰硫脲衍生物的合成与表征

新型2－乙内酰硫脲衍生物的合成与表征;乙酰乳酸合成酶;磺酰脲;乙内酰硫脲;合成     

O-烷基,O-芳基硫代磷酰取代硫脲和O-烷基硫代磷酰-双-取代硫脲的研究(Ⅱ)

用硫氰酸钾与硫代磷酰氯制备了硫代磷酰异硫氰基酯和二异硫氰基酯,并以其与不同胺反应,合成了硫代磷酰取代硫脲和硫代磷酰-双-取代硫脲两系列20个新的有机磷化合物,经1HNMR、IR及元素分析确定了它们的化学结构,测定了它们的生物活性。结果表明只有O-异丙基,O-(4-甲基-2-硝基苯基)-N''-萘基硫代磷酰硫脲(PD-1)具有较好的杀菌活性。     

O－烷基，O－芳基硫代磷酰取代硫脲和O－烷基硫代磷酰－双－取代硫脲的研究（Ⅱ）

用硫氰酸钾与硫代磷酰氯制备了硫代磷酰异硫氰基酯和二异硫氰基酯，并以其与不同胺反应，合成了硫代磷酰取代硫脲和硫代磷酰－双－取代硫脲两系列２０个新的有机磷化合物，经~１ＨＮＭＲ、ＩＲ及元素分析确定了它们的化学结构，测定了它们的生物活性。结果表明只有Ｏ－异丙基，Ｏ－（４－甲基－２－硝基苯基）－Ｎ＇－萘基硫代磷酰硫脲（ＰＤ－１）具有较好的杀菌活性。     

N，N＇－硫代磷酰基芳酰胺基硫脲的合成及生物活性

Ｎ，Ｎ＇－硫代磷酰基芳酰胺基硫脲的合成及生物活性金桂玉，解敏雨，赵国锋（南开大学元素有机化学研究所天津３０００７１）关键词芳酰肼，硫代磷酰基异硫氰酸酯，硫代磷酰基芳酰胺基硫脲，合成，生物活性含（硫代）磷酰基的硫脲衍生物具有广泛生物活性，如杀虫［１，２...     

1-脱氢松香酰基-3-芳酰胺基硫脲及其1,3,4-噻二唑类衍生物的合成及抑菌活性

脱氢松香酸;脱氢松香酰基芳酰胺基硫脲;芳基脱氢松香酰胺基噻二唑;抑菌活性     

O—烷基苯基硫代磷酰取代硫脲的合成（Ⅲ）：含P—C键化合物的…

利用Ｏ－烷基苯基硫代磷酸酸异硫氰基酯与胺与胺的加成反应，合成了两系列Ｏ－烷基苯基硫代磷酰取代硫脲化合物，经元素分析、ＩＲ和＾１ＨＮＭＲ确定了它们的结构，并进行了除草活性的测试。     

1-(5-苄基四唑-2-乙酰基)-4-芳酰胺基硫脲及其环化产物的合成

本文合成了一系列新的1-(5-苄基四唑-2-乙酰基)-4-芳酰胺基硫脲(2)。2在8%NaOH溶液作用下, 环化为3-(5-苄基四唑-2-亚甲基)-4-芳酰基-1,2,4-三唑啉-5-硫酮(3)。     

对二甲基氨基苯甲酰胺基硫脲用于苯甲醛的荧光光度法测定

对二甲氨基苯甲酰胺基硫脲(DMABATU)与苯甲醛反应生成发强荧光的席夫碱,该反应用于苯甲醛的定量测定.在pH 5.30 NaAc-HAc缓冲溶液中(含乙腈20%),苯甲醛浓度在1.25×10-7～3.23×10-6 mol/L范围内与荧光强度呈良好的线性关系,方法检出限为3.75×10-8 mol/L,具有相似反应功能团的物质如甲醛、乙醛、丙酮及苯乙酮的存在均不干扰其测定,表现出较好的选择性.该方法应用于废水中苯甲醛的测定,回收率为97.0%～98.5%.     

1—芳酰基—4—取代吡唑甲酰基氨基硫脲和环化产物的合成及生…

利用１－苯基－３－甲基－５－氯－４－吡唑甲酰基异硫氰酸酯（１）与芳酰肼（Ⅱ）的加成反应合成了系列新的酰胺基硫脲衍生物（Ⅱ）并将Ⅲ在酸性条件下进行环化反应得到２－取代吡唑甲酰基氨基５－芳基－１，３，４－噻二唑（Ⅳ）生物活性测定结果表明部分化合物Ⅲ和Ⅳ具有较好的除草活性。     

苯磺酰硫脲衍生物的无溶剂合成

等物质的量的苯磺酰胺钠盐与异硫氰酸酯在封管中、无溶剂和130℃条件下反应,得到一系列苯磺酰硫脲衍生物,产率高到中等.产物结构通过IR,1H NMR,13CNMR,ESI-MS和元素分析的表征.     

Condensation of pseudothiohydantoin with substituted isatins

Pseudothiohydantoin C⁵-mono(hydroxymethyl) derivatives were obtained by the reaction of unsubstituted pseudothiohydantoin with substituted isatins.     

Studies on azolidones and their derivatives

The action of a concentrated aqueous solution of ammonia on 4-thioxothiazolid-2-one has given an isomer of pseudothiohydantoin, 4-iminothiazolid-2-one (I). 5-Substituted derivatives of I have been obtained by the condensation of 1 with carbonyl and nitroso compounds and 4-substituted derivatives by condensation with amino compounds.     

5-azo derivatives of rhodanine and its analogues in the analytical chemistry of the noble metals

Progress in the synthesis and theoretical study of the 5-azo derivatives of rhodanine, thiorhodanine, 3-aminorhodanine, thiohydantoin, pseudothiohydantoin, thiopropiorhodanine, and selenoisorhodanine is discussed. Emphasis is placed on peculiarities in the interaction of this series of reagents with noble metals and their practical application in analytical chemistry.     

The reaction of diethyl oxalate with some azolidones

The condensation of thiazolidine-2, 4-dione, rhodanine, isorhodanine, 2-thiohydantoin, and pseudothiohydantoin with diethyl oxalate has given products which are azolidone-5-glyoxalic acids or their esters. In these compounds, the glyoxalic acid residue is readily replaced under the action of diazonium salts, aromatic nitroso compounds, and aromatic aldehydes with the formation of 5-arylazo-, 5-arylimino-, and 5-arylideneazolidones. 5-Arylidenerhodanines are also formed from 5-isopropylidene-and 5-(β-acetyl-α-methylethylidene)rhodanines by their reaction with aromatic aldehydes and ketones.     

Unexpected complexation of allylpseudothiohydantoin hydrochlorides towards CuX (X = Cl,NO3, ClO4, BF4, 1/2SiF6). The first known examples of joint CuI(Cl,ClO4) and CuI(Cl,BF4) π-complexes

By means of alternating current-electrochemical synthesis starting from a mixture of 2-imino-3-(prop-2-en-1-yl)-1,3-thiazolidin-4-one (3-allylpseudothiohydantoin, napt) and 2-allylamino-1,3-thiazol-4(5H)-one (allylaminopseudothiohydantoin, aapt) hydrochlorides and corresponding copper(II) salts five new π-complexes, [Cu(napt)Cl] (1), [Cu₂(aapt)₂Cl]NO₃ (2), [Cu₂(aapt)₂Cl]BF₄ (3), [Cu₂(aapt)₂Cl]ClO₄ (4) and [Cu₂(aapt)₂Cl]₂SiF₆·2H₂O (5), were obtained and studied by X-ray single crystal diffraction and IR-spectroscopy. Napt and aapt molecules are selectively coordinated to Cu⁺ depending on the anion type. In crystals of 1 and 5, the organic ligands are attached to the metal in a chelating N,(C=C)-bidentate mode. The aapt molecule in 2-4 acts as a tridentate chelating ligand, being coordinated to the copper(I) ion through the heterocyclic N atom, carbonyl O atom, and C=C bond of allyl group, forming an original cationic [Cu₂(aapt)₂Cl]⁺ fragment with both a bridging Cl^– ion and O atom of the C=O group. In the presence of the doubly charged SiF₆^2– anion, Cu(I) in 5 prefers to be bonded with two bridging Cl^– ions, rather than the C=O group, causing [Cu₂(aapt)₂Cl]⁺ units to associate into the infinite cationic chains. Crystals of 3 and 4 are the first known examples of the simultaneous BF₄^–/Cl^– or ClO₄^–/Cl^– participation in copper(I) π-complex formation.     

The reaction of diethyl oxalate with some azolidones

The condensation of thiazolidine-2, 4-dione, rhodanine, isorhodanine, 2-thiohydantoin, and pseudothiohydantoin with diethyl oxalate has given products which are azolidone-5-glyoxalic acids or their esters. In these compounds, the glyoxalic acid residue is readily replaced under the action of diazonium salts, aromatic nitroso compounds, and aromatic aldehydes with the formation of 5-arylazo-, 5-arylimino-, and 5-arylideneazolidones. 5-Arylidenerhodanines are also formed from 5-isopropylidene-and 5-(-acetyl--methylethylidene)rhodanines by their reaction with aromatic aldehydes and ketones.     

A Novel N-Tert-Butyl Derivatives of Pseudothiohydantoin as Potential Target in Anti-Cancer Therapy

Tumors are currently more and more common all over the world; hence, attempts are being made to explain the biochemical processes underlying their development. The search for new therapeutic pathways, with particular emphasis on enzymatic activity and its modulation regulating the level of glucocorticosteroids, may contribute to the development and implementation of new therapeutic options in the treatment process. Our research focuses on understanding the role of 11β-HSD1 and 11β-HSD2 as factors involved in the differentiation and proliferation of neoplastic cells. In this work, we obtained the 9 novel N-tert-butyl substituted 2-aminothiazol-4(5H)-one (pseudothiohydantoin) derivatives, differing in the substituents at C-5 of the thiazole ring. The inhibitory activity and selectivity of the obtained derivatives in relation to two isoforms of 11β-HSD were evaluated. The highest inhibitory activity for 11β-HSD1 showed compound 3h, containing the cyclohexane substituent at the 5-position of the thiazole ring in the spiro system (82.5% at a conc. 10 µM). On the other hand, the derivative 3f with the phenyl substituent at C-5 showed the highest inhibition of 11β-HSD2 (53.57% at a conc. of 10 µM). A low selectivity in the inhibition of 11β-HSD2 was observed but, unlike 18β-glycyrrhetinic acid, these compounds were found to inhibit the activity of 11β-HSD2 to a greater extent than 11β-HSD1, which makes them attractive for further research on their anti-cancer activity.     

两种水产品中农药多残留分析的样品前处理方法及其在111种农药和相关化学品残留同时检测中的应用

建立了两种针对水产品中农药多残留分析的快速样品前处理方法,并将其应用于111种农药及相关化学品残留检测。在样品前处理方法Ⅰ中,样品经丙酮-乙酸乙酯-正己烷(体积比为1∶1∶1)混合溶剂提取,乙腈转溶;在样品前处理方法Ⅱ中,样品用乙腈-水溶液均质,超声波辅助提取,液-液分配。两种方法所得到的提取液分别用Envi-18柱和PSA柱净化后进行气相色谱-质谱(GC-MS)分析。采用选择离子扫描(SIM)方式,外标法定量。该方法简便、快速,在优化的样品前处理条件和GC-MS分析条件下,方法的检出限(S/N=3)为0.001～0.026 mg/kg;在加标水平为0.25 mg/kg时,采用方法Ⅰ时的回收率为72%～113%,相对标准偏差（RSDs）为3.4%～12.1%;采用方法Ⅱ时的回收率为51%～127%(其中回收率为70%～120%的占94%),RSDs为3.2%～13.8%。     

High-throughput measurements of ciprofloxacin,clomipramine and fexofenadine hydrochlorides with an 8-channel electrical titrator

By employing a developed automatic eight-channel electrical titrator, ciprofloxacin, clomipramine and fexofenadine hydrochlorides are determined in batch, respectively, with satisfactory accuracy and precision. It shows a higher efficiency superior to traditional titration method, and maximally 30 measurements per minute can be completed.     

婴幼儿低发锌、铜、铁、钙与疾病的关系探讨

对846例低发锌、456例低发铜、488例低发铁以及595例低发钙婴幼儿与疾病的关系进行了探讨。结果显示,低发锌婴幼儿中反复呼吸道感染、食欲不振和异食癖的患病率分别为71.16%、57.57%和11.47％;低发铜和低发铁婴儿的贫血率分别为15.79%和73.16%,呼吸道感染的患病率分别为9.43%和35.66%：低发钙者中佝楼病的发病率为81.51%。