制备3-O-去红霉糖红霉素衍生物的新途径

目的 开发一种合成酮基内酯和酰基内酯常用中间体3-O-去红霉糖衍生物的新方法。方法 红霉素9(E)-（O-烷基)-肟衍生物与对甲基苯磺酸一水合物在DMF中于室温下反应选择性水解红霉素得到相应的3-O-去红霉糖衍生物。结果 高收率得到3-O-去红霉糖衍生物并利用MS、^13C-NMR、^1H—NMB和IR确定了其结构。结论 该方法是制备3-O-去红霉糖红霉素衍生物的简捷、有效的新途径。     

柔红酮和阿霉酮二肽衍生物的合成

本文报道柔红酮和阿霉酮二肽衍生物的合成。二肽与柔红酮在DCC/DMAP或苯磺酰氯/吡啶存在下反应,得到柔红酮衍生物,继之溴化、水解得到阿霉酮衍生物或直接由二肽与保护阿霉酮酯化,脱保护后得到阿霉酮衍生物。合成的18个化合物对L₁₂₁₀白血病细胞增殖均有抑制作用,并存在一定的构效关系,游离氨基的位置与抗肿瘤活性相关。     

(9S)-红霉胺合成工艺的改进

目的改进地红霉素关键中间体(9S)-红霉胺的合成工艺。方法以红霉素为原料,经亲核加成、重氮化、氢化三步合成(9S)-红霉胺。结果优化工艺后,(9S)-红霉胺总收率为45.8%。结论改进后的方法成本低,操作简单,适合工业化生产。     

柔红酮和阿霉酮二肽衍生物的合成

本文报道柔红酮和阿霉酮的二肽衍生物的合成。二肽与柔红酮在双环己基碳二亚胺——4-二甲氨基吡啶或苯磺酰氯——吡啶存在下反应,可得到柔红酮衍生物。继之溴化、水解得到阿霉酮衍生物或直接由二肽与保护阿霉酮酯化、脱保护后得到。 合成的十八个化合物对L1210白血病细胞增殖均有抑制作用,并存在一定的构效关系。游离氨基的位置与抗肿瘤活性相关,其中N-端以α位氨基活性较强。     

超声波作用下NaBH4/ZrCl4还原9(E)-红霉素肟制备9(S)-红霉胺

9(S)-红霉胺是合成地红霉素和CP-544372的中间体，此化合物可在超声波的作用下利用NaBH4／ZrCl4于室温下还原9(E)-红霉素肟制得，收率为69％，其结构经IR、NMR和MS确证。该方法是制备9(S)-红霉胺的方便、有效的途径。     

超声-微波辐射法合成5-氯苯并三氮唑衍生物

摘 要 目的： 采用超声-微波辐射法合成新的5-氯苯并三氮唑衍生物,并对其结构进行表征。方法: 以5 氯苯并三氮唑为起始原料,与氯乙腈合成中间体,再分别与6-氯烟醛和5-甲醛-2-甲氧基吡啶合成相应的目标产物。结果:合成得到6个新的5 氯苯并三氮唑衍生物,通过测定熔点、IR、LC-MS和¹H-NMR确认其结构。结论: 用超声 微波辐射法合成得到6个5-氯苯并三氮唑衍生物。     

微波辅助合成N-苯氧乙基苯磺酰胺类衍生物

目的 用微波反应合成了一系列N-苯氧乙基苯磺酰胺类衍生物.方法 以N,N-二甲基甲酰胺(DMF)做溶剂,在K2CO3和溴化三乙基苄基铵(TEBA)相转移催化剂存在的情况下,利用微波辐射辅助合成N-苯氧乙基苯磺酰胺类衍生物.结果 合成了12个N-苯氧乙基苯磺酰胺类衍生物,并经1HNMR确证结构.结论 与传统的加热方法比较,微波缩短了反应时间,提高了合成产率.     

微波辐射技术合成香豆素-3-甲酸乙酯的研究

目的考察微波辐射方法合成香豆素-3-甲酸乙酯与传统方法合成相比有无优势以及能否在无溶剂条件下采用微波辐射方法合成香豆素-3-甲酸乙酯。方法采用传统与微波辐射两种方法,在有机碱的催化作用下经Knovengel反应得到相应产物,其结构经IR1、HNMR波谱确证。结果反应得到了目标化合物,收率在75%以上。结论微波辐射辅助合成可以缩短反应时间,提高反应效率,且可以节省溶剂。     

微波及离子液体条件下香豆素类化合物的合成研究

目的：探索操作简便、环境友好的香豆素衍生物的合成方法：方法：以乙酰乙酸乙酯和苯酚类化合物为原料,通过Pechmann反应,在4种不同的反应条件（浓硫酸催化、Lewis酸三氯化铋催化、微波Lewis酸三氯化铋催化、微波离子液体催化）下催化合成多种香豆素衍生物,并对4种方法进行对比。结果：微波离子液体条件下的Pechmann反应与传统方法相比革除了有机溶剂的使用,缩短了反应时间且产率较高。结论：微波及离子液体条件下合成香豆素类化合物是一种条件简单、环境友好的合成方法。     

克拉霉素(利迈先)临床应用进展

克拉霉素(clarithromycin,CLM),化学名为克红霉索、甲红霉索、6—甲红霉素、6—甲氧基红霉素。商品名:克拉先、利迈仙。是半合成的红霉素衍生物(1),是由美国ABBTT公司研制成功。1991年11月美国FDA批准上市。已在美国、日本、英国、意大利、西班牙等20多个国家上市。利迈先是我     

2H-1-苯并吡喃衍生物的合成及其体外抗癌活性的初步评价

目的设计并合成2H-1-苯并吡喃衍生物化合库并对其体外抗癌活性进行评价。方法以2＇-羟基查耳酮为原料通过微波促进合成得到黄酮衍生物中间体，此中间体与POCl，反应得到4-氯-2H-色原烯-3-醛，通过微波辅助液相平行合成的方法，此醛与ROCONHNH2反应得到2H-1-苯并吡喃衍生物化合库。利用HL-60细胞系评价该化合物库的体外抗癌活性。结果与结论合成了含有32个化合物的2H-1-苯并吡喃衍生物库，体外活性评价表明。部分化合物对HL-60细胞的增殖有一定的抑制作用，其中。化合物9e在浓度为30μmol·L^-1的抑制率为70．8％。     

Design,synthesis and biological evaluation of novel quinoline [4,3-b]chromene derivatives as AChE inhibitors through an efficient one-pot,four-component microwave-mediated reaction

An efficient synthesis of chromeno[4,3-b]quinoline derivatives via one-pot, four-component reaction of 4-hydroxycoumarin, formaldehyde, cyclohexanedione, ammonium ceric nitrate under microwave irradiation was accomplished. The structures of these compounds were unambiguously confirmed by single crystal X-ray diffraction. Furthermore, the anti-AChE activities of these compounds in vitro were investigated at concentrations of 20 μM and 50 μM by using a standard Ellman’s method. The relationship of inhibitory activities and structures of these chromeno [4,3-b]quinolines was also systematically studied. Of all the compounds investigated, 4ag emerged as the most potent AChE inhibitor with IC₅₀ values of 5.63 µM, and it might be used as potent lead for the development anti-AChE agents. Moreover, molecular modelling was conducted to understand the optimal interaction of AChE with these types of compounds.     

1-丁基-3-甲基咪唑-L-樟脑磺酸盐催化合成monastrol

目的探索环境友好、操作简便的monastrol合成方法。方法以间羟基苯甲醛、乙酰乙酸乙酯和硫脲为起始原料,在无溶剂微波加热条件下,用绿色室温离子液体1-丁基-3-甲基咪唑-L-樟脑磺酸盐催化Biginelli反应合成monastrol。结果 1-丁基-3-甲基咪唑-L-樟脑磺酸盐在无溶剂微波加热条件下可催化Biginelli反应合成monastrol,操作简单、耗时缩短、环境友好。结论以新型绿色室温离子液体1-丁基-3-甲基咪唑-L-樟脑磺酸盐为催化剂,经微波促进无溶剂Biginelli反应合成monastrol是一种操作简便、反应温和的绿色合成方法。     

哌啶酮类法尼基转移酶抑制药的微波幅射合成与抗肿瘤活性

目的合成设计哌啶酮类法尼基转移酶抑制药，并对其抗肿瘤活性进行初步评价。方法以取代苯甲醛为起始原料，经Perkin反应和Michael加成，最后在微波辐射条件下环合得到目标化合物，并用MTT法测试它们抑制人Hela细胞和ANC-1细胞的IC50值。结果采用微波辐射技术合成哌啶酮类化合物，反应时间为20～45 min，产率为36.0%～67.1%。经1H-NMR、ESI-MS及IR对化合物的结构确证，总共合成11个新化合物。初步抗肿瘤活性测试结果显示11个目标化合物均有抑瘤活性，其中8个化合物IC50值低于氟尿嘧啶。结论哌啶酮类法尼基转移酶抑制药的合成路线可靠，具有显著抗肿瘤活性。     

Microwave-assisted solvent-free synthesis of biologically active novel heterocycles from 3-formylchromones

A series of novel chromone derivatives have been synthesized employing 3-formylchromones and 5-acetyl-1,3-dimethylbarbituric acid as starting materials both under conventional heating method and microwave irradiation technique in good yields. The synthesized compounds were screened in vitro antibacterial activity against the representative panel of two Gram-positive bacteria and two Gram-negative bacteria. The synthesized compounds were also tested for their inhibitory action against three strains of fungus. The various compounds show potent inhibitory action against test organisms.     

吲哚并[3,2-c]喹啉衍生物的微波辅助合成

目的合成吲哚并[3,2-c]喹啉衍生物并优化其工艺。方法微波辅助Michael加成、环合、Fischer吲哚合成。结果合成了6个吲哚并[3,2-c]喹啉衍生物。结论微波能缩短反应时间,提高Michael加成和Fischer吲哚合成反应的收率。     

Synthesis and structure-activity relationships of new 9-N-alkyl derivatives of 9(S)-erythromycylamine

A series of new 9-N-alkyl derivatives of 9(S)-erythromycylamine has been synthesized by reductive alkylation of erythromycylamine with aliphatic aldehydes and sodium cyanoborohydride. Alternative syntheses employing hydrogenation methods have also been developed. These new 9-N-alkyl derivatives possess excellent antimicrobial activity in vitro and in vivo, especially when administered orally to treat experimental infections in mice. From structure-activity studies, 9-N-(1-propyl)erythromycylamine (LY281389) was selected as the most efficacious derivative. These methods have also been extended to the synthesis of some 9-N,N-dialkyl derivatives of erythromycylamine.     

Comparison of Conventional and Microwave-assisted Synthesis of Benzotriazole Derivatives

A green chemistry approach for organic synthesis is described here, which involves microwave exposure of reactants in presence or absence of solvents. A novel and simple method has been developed for the synthesis of some benzotriazole derivatives under microwave irradiation. In addition, these compounds were synthesised also by conventional heating procedures for comparison. All the compounds synthesised were characterised by melting point, TLC, IR and ¹H NMR spectroscopy. Comparison between conventional and microwave-assisted synthesis was done by comparing total reaction time and percentage yield. The results suggest that microwave-assisted syntheses lead to higher yields within very short reaction times. On antifungal evaluation by cup plate method, all compounds showed antifungal activity. One compound showed activity similar to and two compounds showed better activity than standard antifungal drug flucanazole.     

Synthesis and pharmacological properties of some novel pyrazolidine and pyrazole derivatives

Microwave synthesis technique opens new avenues for the synthesis of many compounds. A novel and simple method has been developed for the synthesis of 1-(2,4-dinitrophenyl) pyrazolidine-3,5-dione and 1-(2,4-dinitrophenyl)-3,5-dimethyl-1H-pyrazole derivatives under microwave irradiation. These compounds exhibit mild to moderate antimircrobial activity against different strains of bacteria (e.g. E. coli, P . aeruginosa, S. aureus and B subtilis) and fungi (e.g. C.?albicans and A. niger). All these synthesised compounds have been characterised by employing various techniques like TLC, Elemental analysis, IR, NMR and MS spectra. In addition to this, the yields of these compounds have been compared with the same compounds, obtained by conventional heating procedures. And the results show that by microwave irradiation method, the product yield is either high or may be same but it takes a very short period of time for reaction. Moreover, this technique provides ecofriendly or green chemical pathway for the synthesis of these compounds. Thus, the microwave irradiation method is more useful than the conventional method because of the shorter reaction time, better yield, conservation of energy and ecofriendly nature.