双环笼状磷酸酯衍生物的研究 I: 1-氧代-4-取代-2,6,7-三氧杂-1-磷杂双环[2,2,2]辛烷衍生物的合成和反应研究

用浓硝酸与钒酸盐氧化1-氧代-4-羟甲基-2,6,7-三氧杂-1-磷杂双环-[2,2,2]辛烷(1)得羟酸2. 对应的酰氯3与一系列酚类或芳胺类反应得新化合物4a-4s. 3与苯二酚、氨基酚或苯二胺反应得化合物5a-5e. 研究了3的反应, 并发现4b在醋酸中经铁粉还原时产物发生O→N酰基重排, 通过元素分析、IB、^1H NMR及部分化合物的MS和X射线衍射分析确定了新化合物的结构. 生物初筛正在进行中.     

4-氨基-5-[2-(4-氯苯氧甲基)苯并咪唑-1-亚甲基]-1,2,4-三唑-3-硫酮的核磁共振研究

在无水乙醇和KOH存在下,将2-(4-氯苯氧甲基-1-苯并咪唑乙酰肼(1)与CS2反应,合成出了中间体酰肼二硫代甲酸钾盐.此中间体再与过量的水合肼反应,经环化得到一种新化合物4-氨基-5-[2-(4-氯苯氧甲基)苯并咪唑-1-亚甲基]-1,2,4-三唑-硫酮.采用元素分析、IR及NMR技术确定了新化合物的结构,并利用2...     

双环笼状磷酸酯衍生物的研究 Ⅰ.1-氧代-4-取代-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷衍生物的合成和反应研究

用浓硝酸与钒酸盐氧化1-氧代-4-羟甲基-2,6,7-三氧杂-1-磷杂双环-[2.2.2]辛烷(1)得羧酸2.对应的酰氯3与-系列酚类或芳胺类反应得新化合物4a—4s.3与苯二酚、氨基酚或苯二胺反应得化合物5a—5e.研究了3的反应,并发现4b 在醋酸中经铁粉还原时产物发生 O→N 酰基重排.通过元素分析、IR、~1HNMR 及部分化合物的 MS 和 X 射线衍射分析确定了新化合物的结构.生物初筛正在进行中.     

α-(α’-甲基-卤代苄氧基)-β-(1-咪唑基)-2,4-二氯乙苯硝酸盐的合成与结构表征

先以间二氯苯、氯乙酰氯和咪唑为原料合成β-( 1 -咪唑基 ) -2 ,4 -二氯 -α-苯乙醇 ( ) ,再以二卤苯为原料合成α-氯 -卤代乙苯 ( a～ d) ,然后 , 分别与 a～ d反应 ,生成α-(α -甲基 -卤代苄氧基 ) -β-( 1 -咪唑基 ) -2 ,4 -二氯乙苯硝酸盐 4个新化合物 ,产率分别为 66.8% ,78.5% ,76.8%和 81 .2 % ,新化合物的结构经元素分析 ,IR和 1H NMR表征     

1-氮杂环-2-(6-甲氧基萘-2-基)丙-2-醇的合成、表征与生物活性

6-甲氧基-2-萘基乙酮经硫酸单酯三甲锍环氧化和氮杂环开环反应, 合成了4种新的唑类化合物. 目标物经核磁共振和MS测定其结构; 分析目标物中萘环质子偶合分裂情况, 并确定萘环上各质子的归属. 生物活性测试结果表明, 部分新化合物具有杀菌活性.     

双环笼状磷酸酯的研究(Ⅱ)——1-硫代-1-磷杂-2,6,7-三氧杂双环[2,2,2]辛烷-4-甲撑衍生物的合成

本文合成了1-硫代-1-磷杂-2,6,7-三氧杂双环[2,2,2]辛烷-4-甲撑膦酸酯新化合物11个.发现只有在三乙胺和DMAP同时存在时,1-硫代-1-磷杂-4-羟甲基-2,6,7-三氧杂双环[2,2,2]辛烷方可顺利进行磷酰化得到产物.探讨了DMAP的强有效的催化作用机制.生物初筛表明部分化合物对植物生长有调节作用.     

3-(4-取代-哌嗪-1-甲基)-1,2,3,9-四氢咔唑-4-酮衍生物的合成与止吐活性研究

以1,3-环己二酮(1)为起始原料, 一个羰基与盐酸苯肼发生缩合反应生成1,3-环己二酮单苯腙(2), 2在ZnCl₂催化下通过分子内环合、重排反应得到1,2,3,9-四氢咔唑-4-酮(3), 3的甲基化物4在冰醋酸中经Mannich反应获得其3-二甲胺甲基物5, 5与哌嗪类化合物通过亲核取代反应合成了9个未见文献报道的3-(4-取代-哌嗪-1-甲基)-1,2,3,9-四氢咔唑-4-酮衍生物6a～6i. 所有合成的新化合物均经元素分析、红外光谱、质谱和核磁共振光谱证明其结构; 初步药理试验采用顺铂诱导的大鼠干呕模型研究了新化合物的止吐活性, 结果表明部分新化合物活性与昂丹司琼相当.     

2-芳基-5-(4-硝基苯甲酰氨基)-1,3,4-噻二唑的合成

以芳甲酰肼和对硝基苯甲酰氯为主要原料, 合成出了10个酰氨基硫脲化合物5a～5j, 其中有6个(5d, 5f～5j)为新化合物. 在无需任何酸性催化剂条件下, 将制得的酰氨基硫脲在DMF中加热回流直接脱水关环合成出了9个2-芳基-5-(4-硝基苯甲酰氨基)-1,3,4-噻二唑化合物6a～6i, 其中7个(6b～6d, 6f～6i)为新化合物. 利用IR和1H NMR证明了化合物5存在两种异构体. 目标产物的结构通过IR, 1H NMR和元素分析进行了表征.     

对称-3,3'-二(取代苯基氨基)-4,4'-二(氨基)-5,5'-(1,4-丁二基)-1,2,4-三唑的合成

以己二酸为原料,经酯化、肼解后与异硫氰酸苯酯(或对氯异硫氰酸苯酯)反应合成了两个新化合物——对称-N1,N1'-(1,4-丁二基)二(甲酰胺基)-N4,N4'-二(取代苯基)硫脲(3a和3b);3a和3b分别经肼解合环合成了两个新化合物——对称-3,3'-二(取代苯基氨基)-4,4'-二(氨基)-5,5'-(1,4-丁二基)-1,2,4-三唑,其结构经1H NMR,IR和元素分析表征。     

取代-苄氧基吲哚-3-甲醛-(4''''-硝基)苯腙的合成

以取代苄氧基吲哚-3-甲醛和4-硝基苯肼为原料,乙醇为溶剂,通过缩合脱水反应合成了4个新化合物--取代苄氧基吲哚-3-甲醛-(4'-硝基)苯腙,其结构经1H NMR,IR,MS和元素分析表征.     

Janceolaroside A and janceoside A, two new compounds from the stems and roots of Jasminum lanceolarium

From the stems and roots of Jasminum lanceolarium Roxb., two new compounds, janceolaroside A and janceoside A, have been isolated along with three known compounds, (-)olivil 4'-O-beta-D-glucopyranoside, (+)-cycloolivil-6-O-beta-D-glucopyranoside and syringin. The structures of the new compounds were determined by spectroscopic methods.     

1H and 13C NMR spectral assignments of four dammarane triterpenoids from carnauba wax

The phytochemical investigation of carnauba wax led to the isolation of three new dammarane triterpenoids 1, 2 and 4, together with the known triterpene 3. The structures of the new compounds were determined by 1D and 2D NMR spectroscopy and by comparison with published data for closely related compounds.     

New Isoprenylated Xanthones from Cudrania tricuspidata

A phytochemical investigation of the roots of Cudrania tricuspidata afforded three new isoprenylated xanthones, cudratricusxanthones N–P ( 1 – 3 , resp.), together with five known compounds, 4 – 8 . The structures of the new compounds were elucidated by extensive spectroscopic analyses.     

New sesquiterpenoid and triterpenoids from the fruits of Rhizophora mucronata

A new sesquiterpene (1) and two new pentacyclic triterpenoid esters (2, 3) together with three known compounds (4-6) were isolated from the fruits of Rhizophora mucronata. Their structures were elucidated by analysis of their spectroscopic data. The new compounds were characterized as 3-hydroxy-3,7,11-trimethyl-9-oxododeca-1,10-diene (mucronatone, 1), 3beta-E-caffeoyltaraxerol (2) and 3beta-Z-caffeoyltaraxerol (3).     

Studies on the constituents of the leaves of Baccharis dracunculifolia (Asteraceae) and their cytotoxic activity

A new sesquiterpene, named baccharisketone (1), and a new monoterpene, p-methoxythymol acetate (2), were isolated from the leaves of Baccharis dracunculifolia along with seventeen known compounds (3-19). The structures of the new compounds were determined by spectroscopic means. The growth inhibitory activity of the isolated compounds against leukemia cells (L 1210) was tested and three terpene phenols (4, 6, 17) and five sesquiterpene alcohols (8, 10, 11, 13, 16) were found to exhibit strong cytotoxic activity.     

Five New Terpenes with Cytotoxic Activity from Pestalotiopsis sp.

Five new compounds called Pestalotis A–E (1–5), comprising three monoterpene-lactone compounds (1–3), one tetrahydrobenzofuran derivative (4), and one sesquiterpene (5), were isolated from the EtOAc extract of Pestalotiopsis sp. The structures of the new compounds were elucidated by analysis of their NMR, HRMS, and ECD spectra, and the absolute configurations were established through the comparison of experimental and calculated ECD spectra. All compounds were tested for antitumor activity against SW-480, LoVo, HuH-7, and MCF-7. The results showed that compounds 2 and 4 exhibited potent antitumor activity against SW-480, LoVo, and HuH-7 cell lines. Furthermore, compound 4 was assessed against HuH-7, and the results indicated that the rate of apoptosis was dose-dependent.     

Sesquilignans and dilignans from Campylotropis hirtella (Franch.) Schindl

A new sesquilignan, erythro-Guaiacylglycerol-beta-O-4'-(5')-methoxylariciresinol, together with six known compounds including three sesquilignans and three dilignans, have been isolated from Campylotropis hirtella (Franch.) Schindl. that was used as traditional Chinese medicine for treatment of benign prostate hyperplasia. All these known compounds were found for the first time from the family leguminosae. The structure of the new compound and its relative configurations were elucidated on the basis of detailed spectroscopic analysis (NMR and MS). These compounds showed no obvious inhibition effect on prostate specific antigen secretion in LNCaP cells by ELISA method.     

Terpenoids from Loxocalyx urticifolius

Two new diterpenoids, loxocalyxin A ( 1 ) and 13‐epiloxocalyxin A ( 2 ), and two new sesquiterpenoids, loxocalyxins B and C ( 3 and 4 , resp.), together with three known compounds, were isolated from the MeOH extract of the whole plant of Loxocalyx urticifolius Hemsl . The structures of the new compounds were established by means of spectroscopic analysis including one‐ and two‐dimensional NMR spectroscopy. All new structures were confirmed by X‐ray crystallographic analysis. Their absolute configurations were established.     

3-取代-6-吡唑基-1,2,4-三唑并[3,4-b]-1,3,4-噻二唑类衍生物的合成及生物活性

将5-取代吡唑-3-甲酸乙酯1位甲基化,经水解反应得到3种中间体1-甲基-5-取代1H-吡唑-3-甲酸（2a~2c）;以不同取代的羧酸为原料经一系列反应合成6种中间体3-取代4-氨基-5-巯基-1,2,4-均三唑（3a~3f）;将中间体（2a~2c）和（3a~3f）在三氯氧磷条件下反应,合成出18种1,2,4-三唑并[3,4-b]-1,3,4-噻二唑类化合物(4a~4r),均未见文献报道。 通过IR、1H NMR、13C NMR和元素分析表征了化合物结构。 初步的生物活性测试结果显示,所合成的化合物均表现出不同程度的生长素活性和抑菌活性。 并选取抑菌活性较好的两个化合物进行抗菌药物最低抑菌浓度(MIC)的测定。     

New Isoprenylated Aurones from the Flowers of Rosa damascena

A phytochemical investigation of the flowers of Rosa damascena resulted in the isolation of three new isoprenylated aurones, damaurones C–E ( 1 – 3 , resp.), together with six known compounds, 4 – 9 . The structures of the new compounds were elucidated by spectroscopic methods, including extensive 1D‐ and 2D‐NMR experiments.