2-烷硫基-5-苯基亚甲基-4H-咪唑啉-4-酮的合成与表征

用2-硫代-3-正丁基-5-苯基亚甲基4-咪唑啉二酮的-S-烷基化反应合成了2-烷硫基-3-正丁基-5-苯基亚甲基-4H-咪唑啉-4-酮衍生物。探讨了S-烷基化反应的反应条件和所合成化合物的波谱性质。目标产物均为新的化合物，其结构经元素分析，IR，1H NMR和MS确正。     

2-氨基-4H-咪唑啉-4-酮衍生物的快速平行合成法

咪唑啉酮衍生物是一类具有良好生物活性和药理活性的杂环化合物 [1,2 ] ,尤其是一些 2 -氨基咪唑啉酮表现出良好的杀菌、抗炎及抗癌活性 [3 ,4 ] .从自然界如一些海洋生物中可分离得到含 2 -氨基咪唑啉酮结构的生物碱 [5,6] .最近 ,组合化学方法广泛地应用于有机合成 ,它包括固相合成法和液相合成法[7～ 9] .我们曾应用氮杂 Wittig反应制得 2 -氨基取代咪唑啉酮衍生物 ,部分化合物表现出一定的抑菌活性 [10 ,11] .本文进一步报道应用液相平行反应法快速合成 2 -氨基 - 4H-咪唑啉 - 4-酮衍生物 (4) .该方法应用烯基膦亚胺 1与苯基异氰酸酯的…     

2-硫代-4-咪唑啉二酮的合成与表征

咪唑啉酮衍生物是一类线粒体呼吸抑制剂,对果树黑斑病及由卵菌引起的霜霉病、疫病等的活性很好。2-硫代-5-苯基亚甲基4-咪唑啉二酮衍生物不能用通法制取,其起始原料烯基氨基酸不稳定。本文用三组分串联aza-Wittig堍反应合成2-硫代-3-烷基-5-苯基亚甲基4-咪唑啉二酮类化合物。合成路线如下：     

2-硫代-3-烷基-5-苯基亚甲基-4-咪唑啉二酮衍生物的有效合成新方法

应用烯基膦亚胺与二硫化碳、一级脂肪胺的串联aza-Wittig反应合成了2-硫代-3-烷基-5-苯基亚甲基-4-咪唑啉二酮衍生物。提出了可能的环化反应机理，探讨了所合成化合物的成环反应条件和波谱性质。经元素分析、IR,1H NMR和MS确证产物均为新化合物。     

2-烷基氨基-3-芳基-5-苄基-1-咪唑啉-4-酮的合成及杀菌活性

咪唑啉酮衍生物;反应;2-烷基氨基-3-芳基-5-苄基-1-咪唑啉-4-酮的合成及杀菌活性     

2-对乙酰氨基苯基-4,5-二对硝基苯基咪唑的合成及性能

咪唑化合物;非线性光学活性有机化合物;2-对乙酰氨基苯基-4;5-二对硝基苯基咪唑的合成及性能     

综合型有机化学实验:4,4-二苯基-3-丁烯-2-酮的合成、纯化及表征

以乙酰乙酸乙酯为原料,利用酮羰基选择性保护及去保护的方法,制备4,4-二苯基-3-丁烯-2-酮。实验涉及无水无氧、减压蒸馏和柱色谱层析等操作。该实验合成路线成熟,产物易于纯化且产率高,结合了分子结构的波谱解析,对于学生有机合成实验能力的培养和加深对波谱理论知识的理解和应用,具有很好的教学效果。     

新型2-硫代-5-苯基亚甲基-4-咪唑啉二酮衍生物的合成

研究了用烯基膦亚按与芳基异氰酸酯、硫化钠／冰醋酸的串联aza-Witting反应合成2-硫代-5-苯基亚甲基-4-咪唑啉二酮衍生物的有效方法。提出了可能的环化反应机理，探讨了所合成化合物的成环反应条件和波谱性质。生成的环化产物均为新的化合物，其结构经元素分析、IR，^1H NMR和MS确证。     

5-(4-羟基苯基)-2,4-咪唑啉二酮酯类化合物的合成及其生物活性

在模拟AdSS酶天然抑制剂结构合成5-(4-羟基苄基)-2,4-咪唑啉二酮酯系列化合物的基础上,为优化其结构,以5-(4-羟基苯基)-2,4-咪唑啉二酮为中间体,合成了28个未见文献报道的5-(4-羟基苯基)-2,4-咪唑啉二酮羧酸酯类化合物,它们的结构均经IR,1HNMR和元素分析表征.初步生物活性测试表明目标化合物5-(4-羟基苯基)-2,4-咪唑啉二酮对叔丁基苯甲酸酯(2i)和2-噻吩酸酯(3b)在浓度200μg/mL时对拟南芥生长抑制率达70%..     

新型含2,4-咪唑啉二酮的4-甲基-3-苯基-2-酰亚胺噻唑啉的合成及生物活性

通过酰氯制备异硫氰酸酯,与5-(4-氨基苄基)-2,4-咪唑啉二酮反应合成了含2,4-咪唑啉二酮的N-苯甲酰基-N'-苯基硫脲,然后在三乙胺存在下再与溴丙酮发生碱催化缩合反应以中等以上收率合成了新型含2,4-咪唑啉二酮的4-甲基-3-苯基-2-酰亚胺噻唑啉,它们的化学结构经1H NMR,IR,HR-ESI-MS和化合物3g和4g的X-ray单晶衍射表征,硫脲与溴丙酮的反应机理通过化合物3g和4g的晶体结构得到进一步确证.初步生物活性测定结果表明:部分目标化合物对供试昆虫及菌种显现出良好的抑制活性,如在200 mg/L浓度下化合物3i和4q对小菜蛾的死亡率分别为86%和100%,在50 mg/L浓度下化合物4n对油菜菌核菌的抑制率为82.6%,而它们对油菜和稗草显示出微弱但并不特征的除草活性.     

A rapid and convenient synthesis of 5-unsubstituted 3,4-dihydropyrimidin-2-ones and thiones

A rapid and convenient synthesis of 5-unsubstituted 3,4-dihydropyrimidin-2-ones and thiones was developed. The reaction involves a one-pot reaction between oxalacetic acid, thiourea/urea, and aldehyde under microwave irradiation and provides the products in good yields and much shorter reaction times.     

具有相同简单级数的不同反应类型的半衰期公式

化学反应的半衰期公式不仅与反应级数有关,而且与反应类型相关。具有相同简单级数的不同类型反应的半衰期表达式也往往不一致。对具有简单级数反应的半衰期表达式进行了分析,重点讨论了不同类型的二级反应和三级反应半衰期表达式的特点及其他们之间的内在联系和区别。     

温度和时间对有机合成反应影响的探讨

根据物理化学和有机合成原理,从动力学、热力学、反应机理及溶解度等各方面详细分析了反应温度和反应时间对有机合成反应的影响。通过这些分析,可以让同学们更好地在合成反应课程的学习中掌握和分析反应温度和反应时间对反应的影响。     

Palladium bis(2,2,6,6-tetramethyl-3,5-heptanedionate) catalyzed Suzuki, Heck, Sonogashira, and cyanation reactions

Palladium bis(2,2,6,6-tetramethyl-3,5-heptanedionate): a structurally well-defined O-containing transition metal complex is reported as an efficient catalyst for Suzuki, Heck, and Sonogashira cross-coupling reactions. The protocol was also applied successfully for cyanation of aryl halides under milder operating conditions. The system tolerated the coupling of various aryl halides with alkenes, alkynes, and organoboronic acid along with the cyanation of aryl halides providing good to excellent yields of desired products.     

One-pot and regioselective synthesis of polysubstituted 3,4-dihydroquinazolines and 4,5-dihydro-3H-1,4-benzodiazepin-3-ones by sequential Ugi/Staudinger/aza-Wittig reaction

An efficient one-pot and regioselective synthesis of 3,4-dihydroquinazolines and 4,5-dihydro-3H-1,4-benzodiazepin-3-ones by Ugi/Staudinger/aza-Wittig sequence has been developed. The Ugi reactions of 2-azidobenzylamines, aldehydes, acids (or α-keto acids) and isocyanides produced the azide intermediates, which were then treated with tributylphosphine or triphenylphosphine to give polysubstituted 3,4-dihydroquinazolines or 4,5-dihydro-3H-1,4-benzodiazepin-3-ones in moderate to good yields by tandem Standinger/aza-Wittig reactions.     

Competitive thermal ene reaction and Diels-Alder reactions of 2-[N-(alk-2-enyl)benzylamino]-3-vinylpyrido[1,2-a]pyrimidin-4(4H)-ones

Thermal reaction of 2-[N-(alk-2-enyl)benzylamino]-3-(2-substituted and 2,2-disubstituted)vinylpyrido[1,2-a]pyrimidin-4(4H)-ones gave azepine, the desired ene products, and/or pyran derivatives. The formation of the latter was responsible for the [4+2] cycloaddition reaction between the α,β-unsaturated ester carbonyl moiety as a diene part and the alkenylamino moiety as an ene one. The reaction features depended upon the kinds of substituents both on the vinyl and alkenyl counterparts; strongly electron-withdrawing substituents on the vinyl moiety or an electron-donating substituent on the alkenyl one changed the reaction feature from the ene reaction to the hetero Diels-Alder reaction.     

Traditional and modern approaches to the synthesis of quinoline systems by the Skraup and Doebner-Miller methods. (Review)

Recent data on classical and modified methods for the synthesis of quinoline systems by the Skraup and Doebner-Miller reactions, not included in reviews on heterocycles, are discussed. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 803–824, June, 2006.     

Sulfilimine palladacycles: stable and efficient catalysts for carbon-carbon coupling reactions

A new family of sulfilimine-based palladacycles (1-4) has been synthesized in high yields from easily accessible starting materials and is found to exhibit high catalytic activities for carbon-carbon bond-formation in Suzuki, Heck, Sonogashira and Ullmann-type reactions, affording coupled products in excellent yields.     

Synthesis of substituted biaryls via Suzuki,Stille and Hiyama cross‐coupling and homo‐coupling reactions by CN‐dimeric and monomeric ortho‐palladated catalysts

The catalytic activity of dimeric [Pd{C₆H₂(CH₂CH₂NH₂)–(OMe)₂,2,3}(μ‐Br)]₂ and monomeric [Pd{C₆H₂(CH₂CH₂NH₂)–(OMe)₂,2,3}Br(PPh₃)] complexes as efficient, stable and air‐ and moisture‐tolerant catalysts was investigated in the Suzuki, Stille and Hiyama cross‐coupling and homo‐coupling reactions of various aryl halides. Substituted biaryls were produced in excellent yields in short reaction times using catalytic amounts of these complexes. The monomeric complex was demonstrated to be more active than the corresponding dimeric catalyst for the cross‐coupling reaction of unreactive aryl bromides and chlorides. The combination of homogeneous metal catalysts and microwave irradiation gave higher yields of products in shorter reaction times. Copyright © 2013 John Wiley & Sons, Ltd.     

Synthesis of enantiomerically enriched secondary and tertiary phenylthio- and phenoxy-aldols

α-Phenoxy- and phenylthio-ketones have been explored as donors and acceptors in organocatalytic aldol reactions. Our studies have revealed effective methodologies for accessing structurally varied and enantiomerically enriched secondary and tertiary phenylthio- and phenoxy-aldols, expanding the scope and potential synthetic utility of organocatalytic direct aldol reactions.