共查询到19条相似文献,搜索用时 125 毫秒
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据文献报道,以3-甲氧甲酰基-2,4-二氧哌啶钠盐(2)为原料,采用两条不同的合成路线,成功地制备了盐酸阿洛司琼(alosetron,1)。路线一以化合物2与1-甲基-1-苯肼硫酸盐缩合得到5,6-二氢-4-(2-甲基-2-苯肼)-2(1H)-吡啶酮(3),再经环合、对接制得盐酸阿洛司琼,总收率为10%。路线二以化合物2经脱竣制得2,4-哌啶二酮(5),与1-甲基-1-苯肼缩合制得3,再经环合、对接制得盐酸阿洛司琼,总收率为23.7%。经IR、UV、^1H-NMR、^13C-NMR及MS测试确证目标化合物结构。 相似文献
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为了盐酸昂丹司琼的质控,合成了欧洲药典7.0中规定的有关物质B[6,6′-亚甲基双[9-甲基-3-[(2-甲基-1H-咪唑-1-基)甲基]-1,2,3,9-四氢-4H-咔唑-4-酮]]:用4,4′-二氨基二苯甲烷经重氮化及还原得到4,4′-二肼基二苯甲烷二盐酸盐,与1,3-环己二酮缩合后进行Fischer环合生成6,6′-亚甲基双(1,2,3,9-四氢4H-咔唑-4-酮),再经甲基化、与多聚甲醛进行羟醛缩合反应,最后与2-甲基咪唑进行Michael加成制得. 相似文献
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《中国药物化学杂志》2015,(4)
目的优化盐酸昂丹司琼的合成工艺。方法以1,2,3,9-四氢-4H-咔唑-4-酮为起始原料,经甲基化得9-甲基-1,2,3,9-四氢-4H-咔唑-4-酮(3),3与二甲胺盐酸盐、多聚甲醛、2-甲基咪唑经过"一锅烩"反应得到中间体9-甲基-3-[(2-甲基-1H-咪唑-1-基)甲基]-1,2,3,9-四氢-4H-咔唑-4-酮(4),4经成盐反应得到目标产物盐酸昂丹司琼。结果与结论目标化合物的结构经1H-NM R、M S谱确证,总收率为57.2%,该合成工艺步骤简便,收率较高,易于工业化生产。 相似文献
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以β-氨基丙到为原料,经酯化、酰胺化、环合、水解、缩合、环合、缩合并成盐制得盐酸阿洛司酮,总收率15.6%,并且改进了中间体8和11的提取分离及纯化工艺。操作简便,产品质量得到改善。 相似文献
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Harald Gröger Matthias Pieper Burghard König Thomas Bayer Herbert Schleich 《Sustainable Chemistry and Pharmacy》2017
Reflecting its importance as key intermediate for the large scale manufacture of β-lactam-type antibiotic drugs being widely used in antibacterial therapy, tremendous achievements have been made over the past decades in developing both, economically and ecologically attractive production routes for 7-aminocephalosporanic acid (7-ACA). Representative achievements and industrial landmarks thereof are described in this review. With cephalosporin C a starting material being accessible through fermentation is readily available in bulk quantities. Initially a chemical production process in organic medium based on various reagents for protection group chemistry and acyclic amide activation served as the large scale production technology for transforming cephalosporin C into 7-ACA. Subsequently, a bi-enzymatic production in aqueous reaction medium based on the use of a D-amino acid oxidase for side chain modification and glutaryl acylase for side chain cleavage was developed. This biocatalytic approach also turned out as an industrial scale solution and dramatically reduced the amount of waste from 31 kg (for the "original chemical process") to less than 1 kg. The latest innovation has been the extension of the two-step bi-enzymatic process towards a one-step monoenzymatic process based on a direct cleavage of the acyclic amide bond of cephalosporin C by means of a cephalosporin C acylase. This alternative, economically efficient and sustainable biotechnological process has already been established on industrial scale in recent years. These biotechnological achievements represent industrial landmarks in biocatalysis and examples that modern biocatalysis can contribute to the development and implementation of highly economical as well as sustainable industrial manufacturing processes. 相似文献
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膜分离技术制备植酸的研究 总被引:7,自引:0,他引:7
应用离子交换与膜分离技术制备植酸,产品纯度高达87%,不含高分子化合物,贮存稳定。产品收率从植酸盐法的73.8%提高到86.4%,成本也随之下降。本法操作简便,生产自动化程度高,尤适于较大规模生产。 相似文献
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司氟沙星合成工艺研究 总被引:8,自引:3,他引:5
司氟沙星由2,3,4,5-四氟苯甲酸经硝化、酰氯化、缩合、环合、还原、水解、酰化,再与顺式2,6-二甲基哌嗪缩合、水解而得,工艺简便,反应条件温和,可用于工业化生产。 相似文献
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托品酸(tropic acid,3-羟基-2-苯丙酸,1)是山莨菪碱(anisodamine)和托吡卡胺(tropicamide)的重要中间体。可由苯乙酸甲酯(2)和甲酸乙酯在醇钠作用下缩合得到的a-甲酰基苯乙酸甲酯经KBH4还原得托品酸甲酯(3),然后碱性水解得到,收率56%(全国原料药工艺汇编,1980. 1141)。本文用2和多聚甲醛在碳酸氢钠作用下缩合直接得到3[1],再经水解得到1(图1),操作简便,收率67.8%。实验部分托品酸甲酯(3)室温及氮气保护下将碳酸氢钠(0.17g,2mmol)、多聚甲醛(2.8g,0.09mol)、二甲亚砜(16ml)和苯乙酸甲酯(12g,0.08mol)混合后缓慢升温至34℃,保温反应1h后升温… 相似文献
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目的 优化酒石酸唑吡坦的合成工艺.方法 以6-甲基-2-(4-甲基苯基)-咪唑并[1,2-α]吡啶为起始原料,通过缩合、还原、甲酯化、胺解、成盐5步反应合成酒石酸唑吡坦.结果 酒石酸唑吡坦总收率由30% ~ 35%提高到45%左右,副反应少,杂质简单.结论 优化后的合成工艺,操作简单、易行,工艺稳定,可满足工业化生产的要求. 相似文献
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达菲作为预防及治疗禽流感的药物,2009年销售额达到30亿美元的高峰。罗氏公司的科学家以莽草酸代替奎尼酸,改善了达菲最初的生产过程,解决了大规模生产的原料供应问题,而莽草酸原料主要从原产于中国的八角中提取。由于有严密的专利保护,罗氏公司可独享这块市场。由此说明技术创新对医药企业发展的重要性,提示中国经济取得重大发展后,应大力开展医药领域的创新,壮大自己的民族医药企业。 相似文献