The Synthesis of Some Novel N-[α-(Isoflavone-7-O-) Acetyl]Amino Acid Derivatives

IsoflavonoidsarebiologicallyimportantnaturalproductsoccurringmainlyinspeciesoftheLeguminosaefamilyandhaveshownawidespectrumofbiologicalactivitiesincludingestrogenic,anticancer,insecticidal,pisciadalandantifungalproperty'.Theseisoflavonoidphytoestrogensarerichinsomeplantdietsuchassoybean'.Animalexperimentshadshownthatsoybeandietinhibitradiation-andchemical-inducedtumorofthemammary',skin',andlivers.AstudyconductedbyBarnesetal.6suggestedthatsoybeanisoflavonesmayberesponsiblefortheanticarcinogeni…     

Synthesis of propyl O-(α-L-rhamnopyranosyl)-(1→3)-[2,4-di-O-(2s-methylbutyryl)-α-L-rhamno-pyranosyl]-(1→2)-(3-O-acetyl-β-D-glucopyranosyl)-(1→2)-β-D-fucopyranoside,the tetrasaccharide moiety of Tricolorin A

Propyl O-(α-L-rhamncpyranosyl)-(1→3)-[2,4-di-O-(2s-methylbutyryl)-α-L-rham-nopyranosyl]-(1→2)-(3-O-acetyl-β-D-glucopyranosyl)-(1→2)-β-D-fucopyranoside (1), the tetrasac-charide moiety of Tricolorin A, was synthesized in total 23 steps with a longest linear sequence of 10 steps, and overall yield of 3.7% from D-Glucose. The isomerization of the dioxolane-type berzyli-dene in the presence of NIS/AgOTf was observed. Tetrasaccharide 1 exhibited no activity against the cultured P388 cell as Tricolorin A did.     

LC-MS~n测定2-[[(2′-氰基联苯基)-4-基]甲基]氨基-3-硝基苯甲酸乙酯中的不纯物

2-[[(2′-氰基联苯基)-4-基]甲基]氨基-3-硝基苯甲酸乙酯是生产抗高血压药坎地沙坦酯的中间产物[1],由3-硝基邻苯二甲酸为起始原料,经酯化、卤代、Curtius重排、与2-氰基-4′-溴甲基联苯缩合4步反应制得,合成路线见文献[2-3]。在生产过程中,每一步反应带来的副产物都影响到最终     

Synthesis of Certain 3-Aminopyrazolo[5,4-b]pyridine and 3,4-Substituted Pyrido[2′,3′：3,4]pyrazolo[5,1-c][1,2,4]triazine Derivatives

2-Thioxo-1,2-dihydropyridine derivatives 2a, 2b were reacted with methyl iodide to give 2-methylthiopyridines 3a, 3b, which were reacted with hydrazine hydrate to produce 3-aminopyrazolo[5,4-b]pyridines 4a, 4b. Compounds 4a, 4b were diazotized to afford the corresponding diazonium salts 5a, 5b, which were reacted with some active methylene compounds 6a-6h to give the corresponding pyrido[2′,3′ ： 3,4]pyrazole[5,1-c][1,2,4]triazines 7-14.     

含有1H-1,2,4-三唑咪唑[2,1-b]-1,3,4-噻二唑、S-三唑[3,4-b]-1,3,4-噻二唑衍生物的合成及生物活性

合成了18个含有1H-1,2,4-三唑的咪唑[2,1-b]-1,3,4-噻二唑以及S-三唑[3,4-b]-1,3,4-噻二唑的稠杂环衍生物,经元素分析及谱学表征,探讨2,5,6-三取代咪唑[2,1-b]-1,3,4-噻二唑的可能生成机制.对大肠杆菌、绿脓杆菌、枯草杆菌等初步抑菌试验证明,多数化合物表现了较好的抑菌活性.     

Synthesis and Crystal Structure of 4-（4-Bromophenyl）- 3,4-dihydro-6-methyl quinolin-2（1H）-one

The title compound (C16H14BrNO) has been synthesized by the reaction of p-tolylamine, Meldrum’s acid and 4-bromo-benzaldehyde, and its structure was characterized by IR, 1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a = 7.6850(11), b = 8.3004(11), c = 21.301(3) , β = 95.110(2)°, V = 1353.4(3) 3, Mr = 316.19, Z = 4, Dc = 1.552 g/cm3, μ(MoKα) = 3.028 mm-1, F(000) = 640, the final R = 0.0345 and wR = 0.0768. X-ray analysis reveals that the atoms of C(1), C(2), C(3), C(4), C(5) and N(1) form a six-membered ring of boat conformation.     

3-烷基/芳基-6-(2′,4′-二氯苯基)-7H-1,2,4-三唑[3,4-b]-1,3,4-噻二嗪的合成及波谱性质

以间二氯苯与氯乙酰氯反应,生成ω-氯代-2,4-二氯苯乙酮(1),再使之分别与3-烷基/芳基-4-氨基-5-巯基-1,2,4-三唑(2a～2l)反应,合成了12种新的3-烷基/芳基-6-(2′,4′-二氯苯基)-7H-1,2,4-三唑并[3,4-b]1,3,4-噻二嗪(4a～4l).利用EA,IR,1H NMR确定了其结构,并提出该反应的可能机制.     

Synthesis and characterization of α-{3-[2-hydroxy-3-(N-methyl-N-hydroxy-ethylamino)propoxy]propyl}-ω-butylpolydimethylsiloxanes.

α-{3-[2-hydroxy-3-(N-methyl-N-hydroxyethylamino)propoxy]propyl}-ω-butylpolydimethylsiloxanes Ⅲ with various moleculax weights were prepared by epoxy addition of α-[3-(2,3-epoxy-propoxy)propyl]-ω-butylpolydimethylsiloxanes Ⅱ and Nmethylmonoethanolamine.At each step.the outcome compounds were characterized through FT-IR and NMR spectra,the results showed that each step was successfully carried out and objective products were achieved.     

1-[2-(2,4-二氯苯氧)乙酰基]-5-氨基-1H-吡唑衍生物的合成与生物活性

为寻求高效低毒的农药,设计、合成了一系列新的1-[2-(2,4-二氯苯氧)乙酰基]-5-氨基-1H-吡唑衍生物3a～3j和4a～4d.元素分析,1H NMR,IR和MS证实了它们的结构.初步的生物活性测试结果表明,在10 mg/L浓度下,化合物3a～3j和4a～4d对油菜的根茎均有很好的抑制作用,对油菜的根的抑制率为90.0%～98.7%;于100 mg/L浓度下,对稗草的根抑制率为84.0%～100%.     

(4R-cis)-6-[2-[2-(4-氟苯基)-5-(1-异丙基)-3-苯基-4-[苯胺(羰基)]-1 H-吡咯-1-基]乙基]-2,2-二甲基-1,3-二氧己环-4-乙酸叔丁酯的波谱学研究

对(4R-cis)-6-[2-[2-(4-氟苯基)-5-(1-异丙基)-3-苯基-4-[苯胺(羰基)]-^1H-吡咯-1-基]乙基]-2,2-二甲基-1,3-二氧己环-4-乙酸叔丁酯的傅里叶变换离子回旋共振质谱(FT-ICR-MS)、核磁共振氢谱(^1H-NMR)、碳谱(^13C-NMR)以及^1H同核位移相关谱(^1H-^1HCOSY)、检出^1H的异核多量子相干谱(HMQC)和^1H检测的异核多键相关谱(HMBC)报道并进行解析。确定了^1H谱、^13C谱中各谱峰的归属,研究了其六元环部分的立体构象,并就空间效应对其化学位移的影响做了初步的探讨。     

(5S,6R)-2-(4-甲基)苯基-6-[(1R)-叔丁基二甲基硅氧乙基]-青霉烯-3-羧酸乙酯的合成研究

青霉烯[1]类抗生素是近年来发展很快的一种非典型β-内酰胺抗生素.青霉烯类化合物[2]具有广泛的抗菌活性,具有优于碳青霉烯类抗生素的特点,其固体化合物和酯型前药可口服吸收,不易被β-内酰胺酶水解,同时对脱氢肽水解酶-I( DHP-I )较碳青霉烯稳定.     

(E)-2-[2-(6-氯嘧啶-4-基氧基)苯基]-3-甲氧基丙烯酸甲酯的合成工艺改进

以3-(α-甲氧基)亚甲基苯并呋喃-2-(3H)-酮为原料,经3步反应合成了杀菌剂嘧菌酯的重要中间体——(E)-2-[2-(6-氯嘧啶-4-基氧基)苯基]-3-甲氧基丙烯酸甲酯(4),总收率61%。4的结构经NMR表征。     

反相高效液相色谱法测定α-(2-氨基噻唑-4-基)-α-[(叔-丁氧基羰基)异丙氧亚胺基]-乙酸

提出了制备头孢类抗生素的中间体α-(2-氨基噻唑-4-基)-α[(叔-丁氧基羰基)异丙氧亚胺基]-乙酸(ATIA)的反相高效液相色谱测定方法,采用SpherigelTM C18色谱柱(250 mm×4.6 mm,5μm),以0.05 g·L-1四丁基溴化铵的甲醇-水(6+4)溶液为流动相,流速为1 mL·min-1,柱温30℃,检测波长260 nm,以外标法定量.在0.001～1.0 mg范围内,ATIA的质量与峰面积呈线性关系,回归方程为A=31 475.6m+1 786.7,相关系数为0.999 7,以质量为0.06 mgATIA按方法测定6次,算得其相对标准偏差为3.7%,检出限(3S)为0.6μg,回收率的试验结果在98.8%～104.0%之间.     

1,2,4-三唑并[3,4-b]-1,3,4-噻二唑的合成

近年来稠杂环化合物的合成及其生物活性的研究日益成为杂环化学研究的热门课题。3,6-二取代-1,2,4-三唑并噻二唑衍生物是具有广谱生物活性的稠杂环化合物,如抗菌、消炎、杀微生物、调节植物生长、除草等,因而引起各国化学家的广泛兴趣。此类化合物的生物活性,     

Synthesis and electrochemical properties of 2,6-bis（6-aryl-[1,2,4]- triazolo[3,4-b][1,3,4]-thiadiazole-3-yl）pyridines

By the condensation of 2,6-bis（4-amino-5-mercapto-[1,2,4]-triazoles-2）pyridine with aromatic acid in the presence of phosphorus oxychloride. Compounds of 2,6-bis（6-aryl-[1,2,4]-triazolo[3,4-b][1,3,4]-thiadiazole-3-yl）pyridines were synthesized. Their structures were confirmed by IR, ^1H NMR spectroscopies and elemental analysis. Their electrochemical behavior and cyclic voltammogram also were be studied. The results showed that they have high ionization potentials and good affinity.     

新型3-取代-6-(4-氯苯基)-7-(1H-1,2,4-三唑-1-基)-1',2',4'-三唑[3,4-b]-1",3",4"-噻二嗪衍生物的合成及抗菌活性

通过3-取代-4-氨基-5-巯基-1,2,4-三唑(3a～3m)和2-溴-2-(1H–1,2,4-三唑-1-基)-4′-氯代苯乙酮(2)的缩合反应,合成了13个新型3-取代-6-(4-氯苯基)-7-(1H-1,2,4-三唑-1-基)-1',2',4'-三唑[3,4-b]-1",3",4"-噻二嗪衍生物4a～4m.化合物结构经元素分析,1HNMR,IR和MS进行了表征.抗菌试验表明所合成的化合物对细菌表现出中等程度的抑制活性.     

(3aS,6aR)-1,3-二苄基-六氢-1H-噻吩并[3,4-d]咪唑-2,4-二酮制备方法的改进

( )-生物素,又称维生素H或辅酶R,化学名(3aS,4S,6aR)-六氢-2-氧-噻吩并[3,4-d]咪唑-4-戊酸,属于水溶性B族维生素,是整个生物界所必须的。生物素在维持动物正常发育,繁殖及保持皮肤、羽毛和骨骼健康中发挥重要作用。自1949年瑞士Roche公司首次开发化学全合成d-生物素后,经过几十     

超声辐射合成5,7-二取代-2-(5-芳基-2-呋喃甲酰亚胺)-[1,2,4]-噻二唑并[2,3-α]嘧啶衍生物及其生物活性研究

利用相转移催化法在超声辐射下合成了8种未见文献报道的5,7-二取代-2-(5-芳基-2-呋喃甲酰亚胺)-[1,2,4]-噻二唑并[2,3-α]嘧啶衍生物.其结构经元素分析、IR和1H NMR得到确证.该法具有操作简便,反应时间短等优点.初步的生物活性测试结果表明部分化合物具有一定除草活性.     

稠杂环化合物的研究(Ⅷ)——3-(α-萘亚甲基)-6-烷基/芳基均三唑并[3,4-b]-1,3,4-噻二唑的合成及生物活性研究

合成了15个新的3-(α-萘亚甲基)-6-烷基/芳基均三唑并[3,4-b]-1,3,4-噻二唑,经EA、JR、~1H NMR和MS确定其组成和结构,并对其代表物4b、4d、4f和4g的抗菌、除草、植物生长调节活性进行了初步观察。     

Synthesis and Crystal Structure of 2-p-Methyloxyphenyl- 3a-（2-phenyl-1,2,3-triazole-4-yl）-3,4-dihydro-1,2,4- oxa-diazolo[4,5-d][1,5] Benzothiazepine

The title compound2-p-methyloxyphenyl-3a-(2-phenyl-1,2,3-triazole-4-yl)-3,4- dihydro-1,2,4-oxa-diazolo[4,5-d][1,5] benzothiazepine (C31H25N5O2S, Mr = 531.63) has been syn- thesized and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1 with a = 10.888(2), b = 15.115(3), c = 16.702(3), α = 99.90(3), β = 95.21(3), γ = 100.41(3)o, V = 2642.1(9) nm3, Dc = 1.336 g/cm3, Z = 4, F(000) = 1112, μ = 0.162 mm-1 ,λ(MoKα) = 0.071073 nm, R = 0.0357 and wR = 0.1126 for 10620 observed reflections with I > 2σ(I). X-ray analysis reveals that the molecular backbone consists of a tricyclic system with the central seven- membered ring in a twisted boat-like conformation.