含(1-芳乙酰胺基-2-叔胺基)乙烷结构的六氢-1H-1,4-二氮革类新化合物的合成(Ⅱ)

设计并合成了2-[1-(4-(N-苯基-N-丙酰基)氨基)哌啶基]甲基-六氢-1H-1,4-二氮 7.由3经还原、氯取代、胺取代、胺脱苄反应得到了7.7经单酰化反应得到了8.8经酰化反应后得到了11个带有(1-芳乙酰胺基-2-叔氨基)乙烷结构的六氢-1H-1,4-二氮类目标化合物(9a～9g,10a～10d).     

含(1-芳乙酰胺基-2-叔胺基)乙烷结构的六氢-1H-1,4-二氮类新化合物的合成(Ⅰ)

合成了 N,N -二苄基 -2 -甲氧羰基 -六氢 -1 H-1 ,4 -二氮 艹卓 (3 )。 3经还原、氯取代、胺取代、胺脱苄、单酰化及酰化反应后得到了 1 0个带有 (1 -芳乙酰胺基 -2 -叔氨基 )乙烷结构的六氢 -1 H-1 ,4 -二氮 艹卓 类目标化合物 (9a～9i和 1 0 )     

乙二胺四乙酸-α,ω-双[2-(2-硝基-1H-咪唑)]乙醇二酯的微波合成

氨基乙醛缩二甲醇和S-甲基异硫脲硫酸盐经缩合和环化反应制得2-氨基咪唑硫酸盐(2);2经重氮化-Sandmeyer后与2-溴乙醇经取代反应制得2-(2-硝基-1H-咪唑)乙醇(4);在微波辐射下,4与乙二胺四乙酸二酐经酯化反应合成了新化合物——乙二胺四乙酸-α,ω-双[2-(2-硝基-1H-咪唑)]乙醇二酯,其结构经1H NMR,FT-IR,HR-MS及元素分析表征。     

新型氨基功能化碱性离子液体1-(2-氨基乙基)-3-甲基咪唑咪唑盐催化四类取代2-氨基-4H-色烯衍生物的合成

设计合成了阴阳离子均具有碱性位点的新型氨基功能化碱性离子液体1-(2-氨基乙基)-3-甲基咪唑咪唑盐([2-aemim]im,3),经ESIMS和1H NMR确定了结构.[2-aemim]im的碱性与氨基功能化的阳离子([2-amim]+)有关,但主要取决于咪唑阴离子(im-).TG-DSC分析显示[2-aemim]im具有高的热稳定性.将[2-aemim]im用于催化水相介质中芳香醛、丙二腈和酚的三组分一锅法反应制备2-氨基-4H-色烯衍生物,阴阳离子之间表现出协同促进催化作用.该催化剂具有高效和底物作用范围广的特点,应用不同的酚类及类似物,如1-萘酚、2-萘酚、间苯二酚和环己二酮,以高产率得到了相应的不同官能团取代的2-氨基-4H-苯并[h]色烯(4a～4e),2-氨基-4H-苯并[f]色烯(5a～se),2-氨基-4H-色烯(6a～6e)和2-氨基-4H-四氢色烯(7a～7e)四类2-氨基-4H-色烯衍生物.离子液体至少可以循环使用5次,催化活性无显著降低.     

5-取代-1H-1,2,4-三氮唑-3-羧酸的合成及结构表征

以5-氨基-1H-1，2，4-三氮唑-3-羧酸为原料，经重氮化反应和Sandmeyer反应得到5-X(X=Cl，Br，I，CN)-1H-1，2，4-三氮唑-3-羧酸，通过元素分析、UV，IR，1H NMR和MS对所有产物的结构进行了表征。     

含(1-芳乙酰胺基-2-叔胺基)乙烷结构的六氢-1H-1,4-二氮类新化合物的合成(Ⅰ)

合成了N,N＇-二苄基-2-甲氧羰基-六氢-1H-1,4-二氮 (3).3经还原、氯取代、胺取代、胺脱苄、单酰化及酰化反应后得到了10个带有(1-芳乙酰胺基-2-叔氨基)乙烷结构的六氢-1H-1,4-二氮类目标化合物(9a～9i和10).     

1-(2-氨基-3,5-二氰基-4-芳基-4H-吡喃-6-基)愈创兰烃薁的合成

在醋酸铵作用下,通过1-氰乙酰基愈创兰烃薁、芳香醛、丙二腈的三组分反应,一锅法合成了一系列1-(2-氨基-3,5-二氰基-4-芳基-4H-吡喃-6-基)愈创兰烃薁衍生物.该反应操作简单、条件温和、收率良好.产物结构经NMR,MS,IR及元素分析等得以证实.     

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。     

5-卤代-1H-1,2,4-三氮唑-3-羧酸乙酯及其衍生物的合成

以5-氨基-1H1,2,4-三氮唑-3-羧酸乙酯为原料,经Sandmeyer反应合成了5-X-1H-1,2,4-三氮唑-3-羧酸乙酯(X=C1,Br,I)(1a-1c),1a-1c再分别与α-2′,4′-二氟苯乙酮反应合成了3个5-卤代-1-1H-1,2,4-三氮唑-3-羧酸乙酯衍生物(2a-2c),其结构通过元素分析,IR,UV和^1H NMR进行了表征。     

以1-甲基-1-甲氧基乙基为保护基的一锅法合成5-芳香二酮-1H-四氮唑

报道了5-芳香二酮-1H-四氮唑(2)的一锅合成法,并且首次报道了1-甲基-1-甲氧基乙基作为四氮唑氮原子的保护基团,保护与脱保护反应条件温和,操作简便,收率高,为该类化合物的合成提供了一条捷径.采用该方法共合成6个未见文献报道的5-芳香二酮-1H-四氮唑类新化合物,以用于药理活性筛选.     

1-(1-Phthalazinyl)- and 1-(4methoxyphenyl)-6,6dimethyl-4oxo-4,5,6,7-tetrahydroindazole

2-(1-Phthalazinylhydrazino)methylene-(IIIa) or 2-(1-phthalazinylhydrazino)ethylidene-5,5-dimethyl-1,3-cyclohexanediones (IIIb) were prepared from 1-hydrazinophthalazine and 2 formyl- or 2-acetyldimedone. Cyclization of IIIb in the presence ofp- TsOH gave 1-(1-phthalazinyl)3, 6, 6-trimethyl-4-oxo-4, 5, 6, 7-tetrahydroindazole. Reaction of 4-methoxyphenylhydrazine with 2 formyl- and 2-acetyidimedone gave the corresponding 1-(4methoxyphenyl)-4-oxo-4, 5, 6, 7-tetrahydroindazole. In the case of 2 -formyldimedone the intermediate 2-(4methoxyphenylhydrazinomethylene)-5, 5-dimethyl-1,3-cyclohexanedione was isolated.Riga Technological University, Riga LV-1658. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 5, pp. 708–710, May, 1996. Original article submitted December 31, 1995.     

Synthesis of 4-(1-Adamantyl)- and 4-(1-Adamantylmethyl)-substituted Halothiazoles

1-Adamantyl bromomethyl ketone and 1-adamantylmethyl chloromethyl ketone react with potassium thiocyanate in dimethylformamide to give the corresponding thiocyanatoketones which cyclize under the influence of HCl into 4-(1-adamantyl) and 4(-adamantylmethyl)chlorothiazole respectively. 4-(1-Adamantyl)-2-amino-5-bromothiazole and its N-derivative were synthesized by the reaction of 1-adamantyl dibromomethyl ketone with thioureas and N-substituted thiourea in acetonitrile.     

Molecular and Crystal Structure of 1-(4-Chlorophenyl)- 3- (4-Nitrophenyl)- 1-Triazene

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Expression of 4-1BB and 4-1BBL in thymocytes during thymus regeneration

4-1BB, a member of the tumor necrosis factor receptor (TNFR) superfamily, is a major costimulatory receptor that is rapidly expressed on the surface of CD4⁺ and CD8⁺ T cells after antigen- or mitogen-induced activation. The interaction of 4-1BB with 4-1BBL regulates immunity and promotes the survival and expansion of activated T cells. In this study, the expression of 4-1BB and 4-1BBL was examined during regeneration of the murine thymus following acute cyclophosphamide-induced involution. Four-color flow cytometry showed that 4-1BB and 4-1BBL were present in the normal thymus and were preferentially expressed in the regenerating thymus, mainly in CD4⁺CD8⁺ double-positive (DP) thymocytes. Furthermore, the CD4^loCD8^lo, CD4⁺CD8^lo and CD4^loCD8⁺ thymocyte subsets, representing stages of thymocyte differentiation intermediate between DP and single-positive (SP) thymocytes, also expressed 4-1BB and 4-1BBL during thymus regeneration but to a lesser degree. Interestingly, the 4-1BB and 4-1BBL positive cells among the CD4⁺CD8⁺ DP thymocytes present during thymus regeneration were TCR^hi and CD69⁺ unlike the corresponding controls. Moreover, the 4-1BB and 4-1BBL positive cells among the intermediate subsets present during thymus regeneration also exhibited TCR^hi/int and CD69^+/int phenotypes, indicating that 4-1BB and 4-1BBL are predominantly expressed by the positively selected population of the CD4⁺CD8⁺ DP and the intermediate thymocytes during thymus regeneration. RT-PCR and Western blot analyses confirmed the presence and elevated levels of 4-1BB and 4-1BBL mRNA and protein in thymocytes during thymus regeneration. We also found that the interaction of 4-1BB with 4-1BBL promoted thymocyte adhesion to thymic epithelial cells. Our results suggest that 4-1BB and 4-1BBL participate in T lymphopoiesis associated with positive selection during recovery from acute thymic involution.     

Synthesis and Anticholinesterase Activity of 3-{[4-Methyl-3-(4-methylpiperazin-1-yl)]pent-1-en-1-yl}-4H-chromen-4-ones

Russian Journal of General Chemistry - A procedure has been developed and optimized for the synthesis of 3-{[4-methyl-3-(4-methylpiperazin-1-yl)]pent-1-en-1-yl}-4H-chromen-4-ones (as...