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《理化检验(化学分册)》2010,(11)
采用反相高效液相色谱法对血清中阿立哌唑及其代谢物脱氢阿立哌唑进行测定。血清样品经乙醚提取,所得提取液再经35℃氮气吹干,残留物经流动相溶解后,用Zorbax-C18色谱柱分离,用紫外检测器于254 nm波长处测定。阿立哌唑及其代谢物脱氢阿立哌唑的线性范围分别为4.0~2 000μg.L-1和4.0~1 500μg.L-1;测定下限(10S/N)均为4.0μg.L-1。相对回收率分别为100.3%~102.7%和93.7%~103.9%;日内和日间相对标准偏差(n=5)均小于7%。 相似文献
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依匹哌唑是首个治疗精神分裂症的多巴胺、部分5-HT1A受体激动剂和5-HT2A受体拮抗剂类化合物,然而其目前的生产路线存在成本高及收率低等缺点。本文在文献方法的基础上,设计了一条合成依匹哌唑的新路线:以4-取代丁腈和7-羟基喹啉-2-(1H)酮为起始原料,经氧烃基化反应得醚化物1,将醚化物1氰基还原得到氨基物2,氨基物2与Boc-双氯乙基亚胺关环得环合物3,环合物3经脱保护得化合物4,化合物4与4-溴苯并噻吩反应得到目标产物依匹哌唑,采用核磁共振和质谱确证了中间体和目标产物的结构,目标产物纯度高达99.30%,且此合成路线具有操作简单、反应易控、原料易得、产物易分离以及环境友好等优点。 相似文献
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现有最唑草酮的合成路线存在成本高、收率低等缺点。本文对唑草酮的合成工艺进行改进和优化,并建立每一步的质量标准。以邻氟苯胺为原料,经“一锅法”完成氨基保护和氯代,然后经水解、重氮化、“一锅法”制三唑啉酮、氟甲基化、硝化、还原、Meerwein芳基化和酯化9步反应,使用HPLC对反应进行中控,以33.37%的总收率(以邻氟苯胺计),99.12%的纯度得到唑草酮。产物与中间体结构经HPLC-MS和NMR确证。该方法原料安全易得、价格低廉,产品的纯度和收率良好,节省反应时间和设备,适合工业化生产。 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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I W Davies M Taylor J F Marcoux J Wu P G Dormer D Hughes P J Reider 《The Journal of organic chemistry》2001,66(1):251-255
Substituted acetic acids and formamides react in the presence of phosphorus oxychloride to yield the vinamidinium hexafluorophosphate salts 5a-d, 6a-d, and 7 in moderate to good unoptimized recrystallized yields (40-67%) as easily handled nonhygroscopic solids. The 1,3-differentially substituted vinamidinium salts 8 was prepared by amine exchange in 81% yield as are the cyclic diazapinium salts 9 and 10 in > 76% yield. The symmetrical 2-chlorovinamidinium 11 was prepared by displacement of 3 in 71% yield. The 2-chlorovinamidinium salts are cleanly reduced to the parent vinamidinium salts 12-16 using HI or PPh3/pTSA in up to 99% assay yield. 相似文献
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褪黑激素的合成与表征 总被引:1,自引:0,他引:1
以吲哚为起始原料,经4步反应合成了褪黑激素(MLT) 吲哚(1)在甲醇中羟基化得到5-羟基吲哚(2),(2)同2-氯乙胺在乙酸乙酯中进行胺乙基化反应得到5-羟基色胺(3),(3)与硫酸二甲酯在甲苯中对羟基进行醚化,得到5-甲氧基色胺(4),(4)经乙酰化得到产物MLT,收率80% 相似文献
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以碘甲基化法增长碳链合成了D-葡萄庚酮糖。首先以D-葡萄糖酸内酯为原料,在N-甲基吗啡啉催化下进行三甲基硅烷醚保护,产率95%;然后通过正丁基锂/二碘甲烷生成的碘甲基锂试剂对酯羰基加成增长碳链,再在碱性环境中水解得2,7-脱水-β-D-吡喃葡萄庚酮糖,两步产率62%;最后经稀酸水解合成D-葡萄庚酮糖,产率90%(总产率53%)。对D-葡萄庚酮糖和2,7-脱水-β-D-吡喃葡萄庚酮糖的乙酰化产物进行了NMR表征。 相似文献
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Suárez-Castillo OR Meléndez-Rodríguez M Beiza-Granados L Cano-Escudero IC Morales-Ríos MS Joseph-Nathan P 《Natural product communications》2011,6(4):451-456
An efficient route to natural occurring methyl 6-bromoindolyl-3-acetate 1c from methyl indolyl-3-acetate 3 was achieved in 3 steps and 68% overall yield. Thus, in order to regioselectively brominate 3 at the C6-position, introduction of electron withdrawing substituents at N1 and C8 was affected to give intermediate 4 in 82% yield. Bromination of 4 with 8 equiv of bromine in CCl4 and washings with aqueous Na2SO3 gave 5 in 86% yield, which was N- and C-decarbomethoxylated by treatment with NaCN in DMSO, affording 1c in 97% yield. The regioselectivity of bromination was evidenced by NMR spectroscopy and X- ray diffraction analysis. 相似文献
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An enantioselective synthesis of the natural antiproliferative agent quinocarcin was achieved by the directed condensation of optically active alpha-amino aldehyde intermediates. Condensation of the N-protected alpha-amino aldehyde 1, prepared in eight steps (19% yield) from (R,R)-pseudoephedrine glycinamide, with the C-protected alpha-amino aldehyde derivative 2, prepared in seven steps (34% yield) from (R,R)-pseudoephedrine glycinamide, afforded the corresponding imine in quantitative yield. Without isolation, direct treatment of this imine intermediate with 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) and hydrogen cyanide led to cleavage of the fluorenylmethoxycarbonyl (Fmoc) protective group followed by addition of cyanide (Strecker reaction) to form the bis-amino nitriles 3 as a mixture of diastereomers, in 91% yield. Treatment of the diastereomers 3 with trimethylsilyl cyanide and zinc chloride in 2,2,2-trifluoroethanol at 60 degrees C led to stepwise cyclization to form the tetracyclic product 4 (42% yield from 1 and 2). The latter intermediate was transformed into (-)-quinocarcin (1) in five steps (45% yield). The yield of quinocarcin was 19% from 1 and 2 (7 steps), and 4% from pseudoephedrine glycinamide (15 steps). 相似文献