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1. 发明申请

WO2007094886A3 ONE POT SYNTHESIS OF TETRAZOLE DERIVATIVES OF SIROLIMUS 审中-公开
标题翻译：一锅法合成四螺旋四唑衍生物
公开(公告)号：WO2007094886A3
公开(公告)日：2007-11-29
申请号：PCT/US2006061909
申请日：2006-12-12
申请人： ABBOTT LAB , DHAON MADHUP , HSIAO CHU-NUNG , PATEL SUBHASH , BONK PETER , CHEMBURKAR SANJAY , CHEN YONG
发明人： DHAON MADHUP , HSIAO CHU-NUNG , PATEL SUBHASH , BONK PETER , CHEMBURKAR SANJAY , CHEN YONG
IPC分类号： C07D498/18 , A61K31/395
CPC分类号： C07D498/18
摘要： A single-step, one-pot process to obtain zotarolimus and other rapamycin derivatives on large scale that improves currently available syntheses. In one embodiment, dried rapamycin is dissolved in isopropylacetate . After cooling and 2,6-Lutidine addition, triflic anhydride is slowly added at -30° C. Salts are removed by filtration. Tetrazole, followed by a tert-base diisopropylethylamine is added. After incubation at room temperature, the product is concentrated and purified by a silica gel column using THF/heptane as eluant. The product is collected, concentrated, and purified using an acetone/heptane column. The product-containing fractions are concentrated. The product is dissolved in t-BME and precipitated with heptane. The solids are dissolved in acetone, treated with butylated-hydroxy toluene, and the solution concentrated. The process is repeated twice with acetone to remove solvents. At least one stabilizing agent is added, such as BHT at 0.5% before drying.
摘要翻译：大规模获得zotarolimus和其他雷帕霉素衍生物的单步一锅法工艺，改进了目前可用的合成方法。在一个实施方案中，将干燥的雷帕霉素溶解在乙酸异丙酯中。冷却并加入2,6-二甲基吡啶后，在-30℃缓慢加入三氟甲磺酸酐。过滤除去盐。加入四唑，然后加入叔丁基二异丙基乙胺。在室温下温育后，将产物浓缩并通过硅胶柱使用THF /庚烷作为洗脱液进行纯化。收集产物，浓缩并使用丙酮/庚烷柱纯化。含产物的级分被浓缩。将产物溶解在t-BME中并用庚烷沉淀。将固体溶于丙酮中，用丁基化羟基甲苯处理，浓缩溶液。该过程用丙酮重复两次以除去溶剂。在干燥前加入至少一种稳定剂，例如0.5％的BHT。

2. 发明申请

WO2007094886A2 ONE POT SYNTHESIS OF TETRAZOLE DERIVATIVES OF SIROLIMUS 审中-公开
标题翻译： SIROLIMUS的四唑衍生物的一个合成
公开(公告)号：WO2007094886A2
公开(公告)日：2007-08-23
申请号：PCT/US2006/061909
申请日：2006-12-12
申请人： ABBOTT LABORATORIES , DHAON, Madhup , HSIAO, Chu-nung , PATEL, Subhash , BONK, Peter , CHEMBURKAR, Sanjay , CHEN, Young
发明人： DHAON, Madhup , HSIAO, Chu-nung , PATEL, Subhash , BONK, Peter , CHEMBURKAR, Sanjay , CHEN, Young
CPC分类号： C07D498/18
摘要： A single-step, one-pot process to obtain zotarolimus and other rapamycin derivatives on large scale that improves currently available syntheses. In one embodiment, dried rapamycin is dissolved in isopropylacetate . After cooling and 2,6-Lutidine addition, triflic anhydride is slowly added at -30° C. Salts are removed by filtration. Tetrazole, followed by a tert-base diisopropylethylamine is added. After incubation at room temperature, the product is concentrated and purified by a silica gel column using THF/heptane as eluant. The product is collected, concentrated, and purified using an acetone/heptane column. The product-containing fractions are concentrated. The product is dissolved in t-BME and precipitated with heptane. The solids are dissolved in acetone, treated with butylated-hydroxy toluene, and the solution concentrated. The process is repeated twice with acetone to remove solvents. At least one stabilizing agent is added, such as BHT at 0.5% before drying.
摘要翻译：单步，一锅法，大规模获得唑他罗莫斯和其他雷帕霉素衍生物，改善目前可获得的合成。在一个实施方案中，将干燥的雷帕霉素溶解在乙酸异丙酯中。冷却后加入2,6-二甲基吡啶，在-30℃下缓慢加入三氟甲磺酸酐。过滤除去盐。加入四唑，然后加入叔 - 碱二异丙基乙胺。在室温下孵育后，将产物浓缩并通过硅胶柱纯化，使用THF /庚烷作为洗脱剂。使用丙酮/庚烷柱收集，浓缩和纯化产物。将含产物的级分浓缩。将产物溶于t-BME中并用庚烷沉淀。将固体溶解在丙酮中，用丁基化羟基甲苯处理，浓缩溶液。用丙酮重复该过程两次以除去溶剂。在干燥前加入至少一种稳定剂，例如0.5％的BHT。

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