CN103709183B - 三氟柳-金属化合物的合成方法 - Google Patents
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Abstract
本发明的三氟柳-金属化合物的合成方法,合成步骤如下:将三氟柳、4-碘吡唑和Cd(NO3)2 .4H2O按摩尔比1︰1︰1混合后溶于水和乙醇溶液中,水与乙醇的体积比为2︰1，三氟柳与无水乙醇的用量比为1毫摩︰50毫升，在80～120°C条件下回流反应48小时,冷却后将其过滤静置,析出无色晶体,过滤,得三氟柳-金属化合物。本发明具有原料用量少、反应时间短、收率高、操作简单等优点。
Description
技术领域
本发明涉及一种物质的合成方法，特别是一种三氟柳-金属化合物的合成方法。
背景技术
三氟柳又名三氟甲基乙酰水杨酸,是一种结构类似于水杨酸的药物,通过不可逆性抑制血小板环氧合酶而减少血栓的生物合成,作为一种抗血小板凝集药,能预防心肌梗死以及稳定或不稳定心绞痛。另一方面,三氟柳的主要代谢物3-羟基-4-三氟苯甲酸(HTB)是血小板环氧合酶的可逆抑制剂,其消除半衰期很长(大约34小时),有利于三氟柳的抗血小板活性。三氟柳和HTB都能通过抑制血小板磷酸二酯酶增加血小板cAMP含量。三氟柳属抗血小板凝聚剂,在预防和治疗血栓栓塞性疾病及并发症上与阿司匹林相比,可同时拮抗环氧合酶和c-AMP磷酸二酯酶的活性,抗血小板聚集能力强,但在治疗剂量时对前列环素生物合成的影响很小,出血的危险性也很小。此外,无机药物作为一个新兴的课题越来越受到人们的关注,其在医疗、医药、生物化学等方面的贡献也越来越突出,随着晶体工程学,超分子合成化学的快速发展,药物晶体形势的发展也受到越来越多的关注。总之,研究三氟柳-金属化合物的结构、特性及生物活性的关系,对深入了解这些金属药物与体内生物大分子作用,治疗疾病的机制及其药理作用具有重要意义。因此,本发明是通过三氟柳作为第一配体,镉的无机盐作为金属源以及4-碘吡唑作为第二配体在水醇溶液中反应得到的化合物。此外,还对该发明物质进行了详细表征。该类配合物结构新颖,至今在相关领域均没有报道。
发明内容
本发明的目的是提供一种方法简单、条件易控制的三氟柳-金属化合物的合成方法。
本发明的三氟柳-金属化合物的合成方法,合成步骤如下:将三氟柳、4-碘吡唑和Cd(NO3)2 .4H2O按摩尔比1︰1︰1混合后溶于水和乙醇溶液中,水与乙醇的体积比为2︰1，三氟柳与无水乙醇的用量比为1毫摩︰50毫升，在80～120°C条件下回流反应48小时,冷却后将其过滤静置,析出无色晶体,过滤,得三氟柳-金属配合物。
本发明的三氟柳-金属化合物的合成方法,所述的回流反应前将混合物溶液的pH值通过1MNaOH或1MHCl溶液调节为4～8。回流反应温度为100°C。
本发明的三氟柳-金属化合物的合成方法,通过三氟柳作为第一配体,镉的无机盐作为金属源以及4-碘吡唑作为第二配体在水醇溶液中反应得到的化合物，此外,本发明还对该发明的物质进行了详细表征，该类化合物结构新颖。本发明具有原料用量少、反应时间短、收率高、操作简单、好控制等优点。
附图说明
图1、化合物的合成路线；
图2、化合物的红外谱图；
图3、化合物的紫外可见光谱图；
图4、化合物的单元图。
结构表征:元素分析测定值(%):C,25.94;H,1.48;N,8.70;理论值(%):C,25.88;H,1.54;N,8.63。红外光谱分析见图2,主要峰归属如下:3083;2911,1672,1626,1580,1508,1432,1375,1337,1268,1210,1176。紫外光谱见图3,主要峰归属如下:π-π*:245nm,LMCT:307nm,339nm。分子结构见图4。
具体实施方式
本发明的三氟柳-金属配合物的合成方法,合成步骤如下:将三氟柳、4-碘吡唑和金属镉盐按摩尔比1︰1︰1混合后溶于水和乙醇溶液中,水与乙醇的体积比为2︰1，三氟柳与无水乙醇的用量比为1毫摩︰50毫升，在80～120°C条件下回流反应48小时,冷却后将其过滤静置,析出无色晶体,过滤,得三氟柳-金属配合物。回流反应前将混合物溶液的pH值通过1MNaOH或1MHCl溶液调节为4～8
其中所述的回流反应前将混合物溶液的pH值通过1MNaOH或1MHCl溶液调节为4～8之间。回流反应温度为100°C。
具体实施例如下：如图1所示：将0.0248g(0.1mmol)三氟柳、0.0308g,(0.1mmol)Cd(NO3)2 .4H2O和0.0193g(0.1mmol)4-碘吡唑混合后溶于10mL水和5ml乙醇的混合溶剂中,搅拌2.5h得到无色溶液，将混合物溶液的pH值通过1MNaOH或1MHCl溶液调节为6，然后放入100℃条件下的低温反应器中反应48小时（2天）,冷却后得到略浑浊的混合物，过滤,将滤液静置,一个星期之后析出无色晶体,得目标产物。对目标产物进行红外光谱、紫外可见光谱和X-射线衍射分析测试，如图2、3、4所示。
配合物表征仪器:C,H,N分析用PE240C型分析仪测定;红外光谱用JASCOFT/IR-480型光谱仪测试（4000-200cm-1）;紫外光谱用JASCOV-570型光谱仪测试（200-1100nm）;晶体结构数据用X-射线衍射分析（APEXIICCD型衍射仪）测试。
本发明具有原料用量少、反应时间短、收率高、操作简单等优点。
Claims (3)
1.一种三氟柳-金属化合物的合成方法,其特征在于：合成步骤如下:将三氟柳、4-碘吡唑和Cd(NO3)2 .4H2O按摩尔比1︰1︰1溶于水和乙醇混合溶液中,水与乙醇的体积比为2︰1，三氟柳与无水乙醇的用量比为1毫摩︰50毫升，在80～120°C条件下回流反应48小时,冷却后将其过滤静置,析出无色晶体,过滤,得三氟柳-金属化合物。
2.根据权利要求1所述的三氟柳-金属化合物的合成方法,其特征在于：所述的回流反应前将混合物溶液的pH值通过1MNaOH或1MHCl溶液调节为4～8。
3.根据权利要求1或2所述的三氟柳-金属化合物的合成方法,其特征在于：回流反应温度为100°C。
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101177398A (zh) * | 2007-12-11 | 2008-05-14 | 南京海陵中药制药工艺技术研究有限公司 | 一种精制三氟柳的方法 |
| CN101503355A (zh) * | 2009-01-21 | 2009-08-12 | 北京欧克兰医药技术开发中心 | 三氟柳合成精制 |
| CN101830918A (zh) * | 2010-04-30 | 2010-09-15 | 中山大学 | 一种多氮唑锌/镉框架材料的合成方法 |
| CN101948478A (zh) * | 2010-09-03 | 2011-01-19 | 天津师范大学 | 含有5-溴代烟酸的镉(ⅱ)配合物及其制备方法 |
| CN102070657A (zh) * | 2010-12-21 | 2011-05-25 | 河南中医学院 | 双邻香兰素缩乙二胺西佛碱过渡金属配合物及制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177398A (zh) * | 2007-12-11 | 2008-05-14 | 南京海陵中药制药工艺技术研究有限公司 | 一种精制三氟柳的方法 |
| CN101503355A (zh) * | 2009-01-21 | 2009-08-12 | 北京欧克兰医药技术开发中心 | 三氟柳合成精制 |
| CN101830918A (zh) * | 2010-04-30 | 2010-09-15 | 中山大学 | 一种多氮唑锌/镉框架材料的合成方法 |
| CN101948478A (zh) * | 2010-09-03 | 2011-01-19 | 天津师范大学 | 含有5-溴代烟酸的镉(ⅱ)配合物及其制备方法 |
| CN102070657A (zh) * | 2010-12-21 | 2011-05-25 | 河南中医学院 | 双邻香兰素缩乙二胺西佛碱过渡金属配合物及制备方法 |
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