2-氨基-3-氰基-4-芳基-4H-苯并[h]苯并吡喃的一步合成

结构;2-氨基-3-氰基-4-芳基-4H-苯并[h]苯并吡喃的一步合成     

2-氰基-3-取代氨基-3-(2-甲基苯基)丙烯酸乙酯的合成和杀菌活性

2-甲基苯甲酰氯与氰乙酸乙酯反应得到2-氰基-3-羟基-3-(2-甲基苯基)丙烯酸乙酯, 经氯化得到2-氰基-3-氯-3-(2-甲基苯基)丙烯酸乙酯, 再用三乙胺处理合成了11个2-氰基-3-取代氨基-3-(2-甲基苯基)丙烯酸乙酯类目标化合物. 生物活性研究表明这类新化合物具有良好的杀菌活性.     

新型2-羟乙基苯并[d]异噻唑-3(2H)-酮脂肪酸酯的合成及其抑菌活性

以苯并[d]异噻唑-3(2H)-酮为原料,通过取代与酯化反应合成了9个未见文献报道的了2-{3-氧代苯并[d]异噻唑-2(3H)-基}乙醇脂肪酸酯(4a～4i),其结构经1H NMR,IR和元素分析表征。初步体外抑菌活性测试结果表明,4对六种实验菌均表现出不同程度的抑菌活性,尤其对革兰氏阳性菌,用药量32μg.mL-1时抑菌率在90%以上。     

1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲的合成及手性晶体结构

对二甲氨基苯甲醛和苯基氨基硫脲缩合反应生成对二甲氨基苯甲醛缩氨基苯硫脲{1-[4-(dimethylamino)ben- zylidene]-4-phenylthiosemicarbazide}, 并从溶液中析出手性晶体. 元素分析、红外光谱、紫外光谱、核磁谱、质谱和X射线衍射测定其组成和结构. 晶体属正交晶系, P2₁2₁2₁空间群, a＝0.77038(14) nm, b＝1.1428(2) nm, c＝1.6726(3) nm, V＝1.4726(5) nm³, Z＝4, D_c＝1.346 g/cm³, F(000)＝632, μ＝0.219 mm^－1, 可观测点精修最终偏离因子: R＝0.0407, wR＝0.1157. 化合物的晶体结构和固态圆二色谱表明化合物在结晶过程中发生单一对映体的手性堆积.     

2-氨基-3-氰基-4-(4-氟苯基)-4H-苯并[h]苯并吡喃的合成和晶体结构

标题化合物与N,N-二甲基甲酰胺(DMF)形成的1:1混合结晶物C20H23FN2OC3H7NO由对氟苯甲醛、丙二腈、-萘酚在六氢吡啶存在下合成并经DMF与水的混合溶剂重结晶而得, 其结构通过元素分析、IR 和1H NMR对化合物进行了表征,用X-射线单晶衍射法测定了该化合物的晶体结构。结果表明,晶体属于单斜晶系,P21/n空间群,a = 6.365(1), b = 10.620(2), c = 29.122(6) ? b = 92.00(1), V = 1967.3(6) ?, Mr = 389.42, Z = 4, Dc = 1.315 g/cm3, m (MoKa) = 0.092 mm-1, F(000) = 816。晶体结构用直接法解出,经全矩阵最小二乘法修正,最终偏离因子R = 0.047, wR = 0.1053。化合物分子中,原子C(1), C(2), C(3), C(4), C(5) 和O(1)形成1个六员环,该六员环中C(1)C(2)键长为1.346(3) 牛砻魑肆被肺焦瓜蟆?     

1,4-双[4-(2-氨基-5-苯基)噻唑基]苯及其聚酰亚胺的合成及性能

以１ ,４ 双（ 苯乙酰基） 苯为原料,合成了新有机二胺化合物———１ ,４ 双［４ （２ 氨基 ５ 苯基） 噻唑基］ 苯,以此二胺或４ ,４’ 二氨基二苯醚和３ ,３’,４ ,４’ 二苯酮四酸二酐反应制备出新型的聚酰亚胺均聚物和共聚物,研究了它们的耐温性能,耐热氧化性能和共聚物经高温裂解后的导电性能等     

微波法合成2-羟乙基苯并[d]异噻唑-3(2H)-酮

以苯并异噻唑-3(2H)-酮(BIT)及氯乙醇为原料微波法合成了2-羟乙基苯并[d]异噻唑-3(2H)酮。考察了氢氧化钠量,氯乙醇用量,反应时间,反应温度对反应的影响,经正交实验设计得到了最佳反应条件,最佳反应条件下收率为83.3%。结果表明,与传统工艺相比,微波技术合成2-羟乙基苯并[d]异噻唑-3(2H)-酮的方法具有操作方便、收率高等特点,具有一定的应用价值。     

2-氰基-3-甲硫基-3-(4-甲基或6-甲基苯并[d]噻唑-2-氨基)丙烯酸酯类化合物的合成和抗病毒活性研究

以氰基乙酸和氰基乙酸乙酯为起始原料,采用活性基团拼接的方法,将苯并噻唑基团引入氰基丙烯酸酯中,设计合成了14个含有苯并噻唑基团的氰基丙烯酸酯(酰胺)类化合物3.所有化合物结构经过1H NMR,13C NMR,红外光谱和元素分析确证,并对所合成的目标化合物3进行了室内抗烟草花叶病毒(TMV)和抗黄瓜花叶病毒(CMV)活性测试.结果表明该类化合物具有一定的抗TMV和抗CMV活性.在0.5 mg/mL时,化合物3b,3c,3d对CMV表现出较好的活体治疗活性,抑制率分别为46.3％,45.1％,43.7％.     

2-{[(2'-氰基联苯基-4-基)甲基]氨基}-3-硝基苯甲酸甲酯的合成

以3-硝基-2-氨基苯甲酸甲酯为原料,经三氟乙酰化、N-烷基化和脱保护反应制得坎地沙坦中间体2-{[(2'-氰基联苯基-4-基)甲基]氨基}-3-硝基苯甲酸甲酯,其结构经~1H NMR,~(13)C NMR和MS(ESI)确证。     

新型N-酰基-7-甲氧基-苯并[4,5]噻唑并[2,3-c][1,2,4]三唑-3(2H)-硫酮的合成及其除草活性

为了寻找新的含苯并噻唑稠杂环农药先导化合物,以2-氨基-6-甲氧基苯并噻唑为起始原料,经肼化、环化和酰基化反应,合成出了14个N-酰基-7-甲氧基苯并[4,5]噻唑并[2,3-c][1,2,4]三唑-3(2H)-硫酮,并利用1H NMR,ESI-MS及元素分析对其结构进行表征.对目标化合物进行初步的除草活性筛选,实验结果表明:在浓度为200 mg/L时,大部分化合物对黄瓜(Cucumis sativus)、小麦(Triticum aestivum)、高粱(Sorghum vulgare)、萝卜(Raphanus sativus)、油菜(Brassica campestris)和稗草(Echinochloa crusgalli)的根和茎的抑制率在85%以上.     

新型2-氨基-呋喃并[2,3-d]嘧啶-4(3H)-酮衍生物的合成及抗肿瘤活性

报道应用aza-Wittig反应,采用易得的原料,在温和的条件下,以78%～90%的产率有效的合成了新型2-氨基-呋喃并[3,2-d]嘧啶-4(3H)-酮衍生物5,其结构经IR,1H NMR,MS和元素分析确认.为进一步得到结构确认,化合物5c经X射线衍射分析证实.运用噻唑蓝(MTT)标准法对化合物5进行了体外抗肿瘤活性的测定,其中5f对肺癌细胞A459的IC50值为18.4μmol/L,显示出潜在良好的抗肿瘤活性.     

New 6-(4-Bromophenyl)-imidazo[2,1-b]thiazole Derivatives: Synthesis and Antimicrobial Activity

Summary.  New 4-alkyl/aryl-1-((6-(4-bromophenyl)-imidazo[2,1-b]thiazol-3-yl)-acetyl)-3-thiosemicarbazides and 3-alkyl/aryl-2-(((6-(4-bromophenyl)-imidazo[2,1-b]thiazol-3-yl)-acetyl)-hydrazono)-4-thiazolidinones were synthesized from 6-(4-bromophenyl)-imidazo[2,1-b]thiazole-3-acetic acid hydrazide. Their structures were elucidated by elemental analyses and spectroscopic data. All compounds were tested for antibacterial and antifungal activities. The antimicrobial activities of the compounds were assessed by the microbroth dilution technique. The compounds were also evaluated for antituberculosis activity against Mycobacterium tuberculosis H₃₇Rv (ATCC 27294); they exhibited varying degrees of inhibition in the in vitro primary screening at 6.25 μg · cm⁻³. The most active compound was 3-(4-nitrophenyl)-2-(((6-(4-bromophenyl)-imidazo[2,1-b]thiazol-3-yl)-acetyl)-hydrazono)-4-thiazolidinone. Corresponding author. E-mail: nurayulusoy@yahoo.com Received December 10, 2001. Accepted (revised) March 1, 2002     

4H-吡啶并[3,2-e][1,3]噻嗪-4-酮嘧啶衍生物的合成

2-氯烟酸异硫氰酸酯在碱性介质中与取代2-氨基嘧啶反应直接得到4H-吡啶并[3,2-e][1,3]噻嗪-4-酮嘧啶. 所合成的6个未见文献报道的目标化合物经IR, ¹H NMR和元素分析证实了其结构, 并对反应可能机理进行了探讨.     

Synthesis of Pyrimidine Conjugates with 4-(6-Amino-hexanoyl)-7,8-difluoro-3,4-dihydro-3-methyl-2H-[1,4]benzoxazine and Evaluation of Their Antiviral Activity

A series of pyrimidine conjugates containing a fragment of racemic 7,8-difluoro-3,4-dihydro-3-methyl-2H-[1,4]benzoxazine and its (S)-enantiomer attached via a 6-aminohexanoyl fragment were synthesized by the reaction of nucleophilic substitution of chlorine in various chloropyrimidines. The structures of the synthesized compounds were confirmed by ¹H, ¹⁹F, and ¹³C NMR spectral data. Enantiomeric purity of optically active derivatives was confirmed by chiral HPLC. Antiviral evaluation of the synthesized compounds has shown that the replacement of purine with a pyrimidine fragment leads to a decrease in the anti-herpesvirus activity compared to the lead compound, purine conjugate. The studied compounds did not exhibit significant activity against influenza A (H1N1) virus.     

5,6-2H-1,2,4-三唑[3,4-b][1,3,4]噻二嗪衍生物的合成及抗癌活性测定

取代苯甲醛与4-氨基-5-(3,4,5-三甲氧基苯基)-1,2,4-三唑-3-硫酮(2)缩合生成5-(3,4,5-三甲氧基苯基)-4-取代苯基亚胺基-1,2,4-三唑-3-硫酮(3),再烷基加成化为新型5,6-2H-1,2,4-三唑[3,4-b][1,3,4]噻二嗪衍生物4.化合物结构经1HNMR 13C NMR,IR以及元素分析确认.采用噻唑兰(MTT)比色法进行化合物抑制人体前列腺癌细胞(PC3)体外活性测试,结果表明所合成的化合物具有不同程度的抑制PC3活性,其中化合物4a在10μmol·L-1浓度下对PC3的抑制率为75.9%.     

Synthesis and Antimicrobial Activity of Some 3-Substituted-5,6-dimethoxy-2,3-dihydrobenzo[d]thiazol-2-one

Sixteen new compounds derived from the 2,3-dihydrobenzo[d]thiazol-2-one template with various side-chains in position-3 were synthesized and evaluated for their antimicrobial activity. Antibacterial and antifungal screening of the compounds prepared showed that 5,6-dimethoxy-3-(2-oxo-propyl)-2,3-dihydrobenzo[d]thiazol-2-one (3g) exhibited the highest activity.     

Synthesis and Crystal Structure of 2-(4''-Methylphenoxy)-5,8,9-trimethyl-3-phenyl Thieno[3'',2'':5,6]pyrido[4,3-d]pyrimidin-4-(3H)-one Hydrochloride

The title compound 2-(4′-methylphenoxy)-5,8,9-trimethyl-3-phenyl thieno[3′,2′:5,6]pyrido[4,3-d]pyrimidin-4(3H)-one hydrochloride (C26H23Cl4N3O2S, Mr = 583.33) has been deter- mined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 14.8442(11), b = 11.5131(8), c = 17.2010(13) (A), β = 113.7250(10)o, V = 2691.3(3) (A)3, Z = 4, Dc = 1.440 g/cm3, S = 1.094, μ = 0.547 mm-1, F(000) = 1200, the final R = 0.0571 and wR = 0.1458. X-ray analysis reveals that the title compound combines with a molecule of dichloromethane by an intramolecular hydrogen bond. The thienopyridine ring is almost coplanar, and the dihedral angle between the thiophene plane and the pyridine plane is 0.6o.     

4-甲基-苯磺酸-2-氧-2-[3-(5-芳基-[1,3,4]噁二唑-2-基)-硫脲]-乙基酯的合成及生物活性研究

合成了12个未见文献报道的4-甲基-苯磺酸2-氧-2-[3-(5-芳基-[1,3,4]噁二唑-2-基)-硫脲]-乙基酯, 其结构经元素分析、¹H NMR和IR确证. 初步活性测试结果表明: 部分化合物有较好的杀菌活性.