共查询到20条相似文献,搜索用时 31 毫秒
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Loughlin WA Jenkins ID Henderson LC Campitelli MR Healy PC 《The Journal of organic chemistry》2008,73(9):3435-3440
An efficient formal synthesis of (+/-)-hyphodermins A and D, metabolites of Hyphoderma radula, has been completed in 12 and 11 steps, respectively. The tricyclic carbon skeleton of enone 6 was rapidly assembled from diester 11 via an alpha brominationn-elimination sequence followed by anhydride formation. Regioselective reduction of the lactone group of enone 6 with LiAlH(t-BuO) 3 gave lactol 15. Lactol 15 was converted in two steps to (+/-)-hyphodermin D, without the need for complex protection-deprotection strategies. Lactol 15 was converted in three steps to (+/-)-hyphodermin A, via the key step of epoxidation of an enone in the presence of a THP lactol. A combination of NMR and ab initio studies suggests that the structures of hyphodermin C and D should be interchanged. 相似文献
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在脂肪酶Lipozyme TL IM的催化下,2,2,5-三甲基-1,3-二氧六环-5-羧酸酐对抗生素西罗莫司的42-位羟基进行区域选择性酯化制得化合物4;4水解后合成了西罗莫司脂化物Temsirolimus,总产率83.7%。其结构经1H NMR和HR-MS确证。 相似文献
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Pyrolysis of isatoic anhydride (3) at 550°C and ca. 1×10−2 torr gave benzoazetinone (1, 80%) as the only product. The existence of 1 was confirmed by low-temperature NMR spectroscopy at −90°C. Above −20°C, 1 was converted to dimer (4, 50%), trimer (5, 22%), and anthranilic acid (6, 12%). Pyrolysis of 3 at 800°C and ca. 1×10−2 torr gave 1-cyanocyclopentadiene (7) in 38% yield. 相似文献
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Yasuyoshi Miki Yosiyuki Aoki Hideaki Miyatake Toshie Minematsu Hajime Hibino 《Tetrahedron letters》2006,47(29):5215-5218
1-Benzenesulfonylindole-2,3-dicarboxylic anhydride was reacted with methyl 1-benzenesulfonylindole-2-acetate to give the corresponding 2-acylindole-3-carboxylic acid as the sole product in high yield, which could be converted to caulersin in four steps. In a similar manner, three isomers A, B, and C were synthesized by reaction of indole-2,3-dicarboxylic anhydrides with methyl indoleacetates. 相似文献
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以靛红酸酐为起始原料,设计并合成了14个结构新颖的吡啶联喹唑啉酮类衍生物。所有化合物经1H NMR、13 C NMR和高分辨质谱(HRMS)表征确证其结构。初步抗菌活性结果显示,该类化合物对水稻白叶枯病菌(Xanthomonas oryzae pv.Oryzae,Xoo)、猕猴桃溃疡病菌(Pseudomonassyringae pv.actinidae,Psa)和玉米纹枯病菌(Rhizoctonia solani,Rs)均表现出一定的抑制活性。其中化合物2-([3,3′-联吡啶]-5-基)-6-氯-3,8-二甲基喹唑啉-4(3 H)-酮(3m)对Rs的抑制活性可达(51.8%)。 相似文献
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对Kaiser报道的以α-紫罗兰酮为原料合成4-氧代-β-紫罗兰酮的方法进行了改进,研究了影响环氧化、开环和氧化的主要因素,探讨了分离纯化方法,其结构经MS、IR、1H-NMR、13C-NMR和元素分析进行了表征。磷钨酸可有效的催化过氧化氢氧化α-紫罗兰酮合成4,5-环氧-α-紫罗兰酮,当磷钨酸/过氧化氢摩尔比为5:100时,收率为85%;4,5-环氧-α-紫罗兰酮在甲醇钠催化下反应生成羟基紫罗兰酮,收率94%,纯度85%;经琥珀酸酐纯化,收率83%,纯度96%;再经异丙醇铝氧化、柱层析分离,4-氧代-β-紫罗兰酮的收率为93%,反应总收率从47.2%提高至61.7%。 相似文献
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Gao X Zhu G Zeng Z Chen W Lin Z Liu Y Xu P Zhao Y 《Rapid communications in mass spectrometry : RCM》2011,25(8):1061-1069
The mass spectral behavior of amino acid methyl ester phosphoramidate derivatives have been investigated using electrospray ionization multistage mass spectrometry (ESI-MS(n)) and moderate theoretical calculations at the B3LYP/6-31G(d) level. A novel methyl group migration to the phosphoryl group with the formation of the intermediate cyclic aminoacylphosphoramidate was found. The proposed structures of the rearrangement ions were confirmed by high-resolution tandem mass spectrometry. A possible mechanism involving the pentacoordinate phosphoric-carboxylic phosphate anhydride was proposed, in which the metal ion coordination with the phosphoryl and carbonyl groups and the intrinsic properties of phosphoryl group might be the key factors responsible for this novel migration. 相似文献
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以氯乙酰氯和对碘苯胺为原料,经酰化合成了4-碘-氯乙酰苯胺,接着与1-甲基咪唑反应得到氯化1-甲基-3-(4-碘苯氨基甲酰甲基)咪唑钅翁,随后在水溶液中发生阴离子交换,合成了1-甲基-3-(4-碘苯氨基甲酰甲基)咪唑四氟硼酸盐;四氟硼酸盐在过氧化氢/三氟乙酸酐体系中氧化得到一种新的离子液体负载的双(三氟乙酰氧基)碘苯试剂1-甲基-3-[4-双(三氟乙酰氧基)碘苯氨基甲酰甲基]咪唑四氟硼酸盐。反应总收率62.3%。试剂没有吸湿性,在空气中长期放置不变质。化学结构用IR、1H NMR、13C NMR、19F NMR和元素分析表征。 相似文献
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[reaction: see text] The intramolecular Diels-Alder reaction between an amidofuran moiety tethered onto an indole component was examined as a strategy for the synthesis of Aspidosperma and Strychnos alkaloids. Furanyl carbamate 13 was acylated using the mixed anhydride 16 to provide amidofuran 12 in 68% yield. Further N-acylation of this indole furnished 17 in 88% yield. Cyclization precursors were prepared by removing the carbamate moiety followed by N-alkylation with the appropriate alkyl halides. Thermolysis of 25 provided the novel tetracyclic ketone 26 in 74% yield. 相似文献
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应用烯基铜锂试剂合成消旋日本丽金龟性信息素徐章煌,黄锦霞,李焰,潘贻罕,蒋济隆,赵建洪(湖北大学化学系武汉430062)(华中理工大学固态电子学系武汉)关键词日本丽金龟,性信息素,烯基铜日本丽金龟成虫对多种树木、观赏植物及农作物危害极大,1976年,... 相似文献
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以靛红酸酐为起始原料,经硝化、还原上保护、氨解开环、环合、卤素交换和脱保护共七步反应合成了氟喹酮(7),其结构经 1H NMR,13C NMR和ESI-MS确证。研究了硝化试剂、溶剂、催化剂等对7收率的影响,结果表明:在使用浓硝酸作为硝化试剂,甲苯,乙腈等为溶剂,Raney-Ni, TBAB等为催化剂时,总收率可达58%,纯度达99%以上。 相似文献
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Mesoionic 4-trifluoroacetyl-1,3-oxazolium-5-olates (1), obtained from the reaction of N-acyl-N-alkylglycines (2) with trifluoroacetic anhydride, react with amidines to give 5-trifluoroacetylimidazoles (3) in moderate yield. The novel ring transformations of 1 into 3 occur via an initial attack of amidines on the C-2 position of the ring. 相似文献