共查询到19条相似文献,搜索用时 109 毫秒
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目的改进盐酸特拉唑嗪的合成工艺。方法以无水哌嗪为起始原料,经酰化、还原、胺化、成盐等反应制得盐酸特拉唑嗪。结果与结论降低了成本,提高了收率,适合工业化生产。 相似文献
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《中国药物化学杂志》2015,(6):450-452
目的合成选择性去甲肾上腺素再摄取抑制剂类抗抑郁药物盐酸维洛沙嗪。方法以2-乙氧基苯酚为原料,经环氧化、胺解、成盐反应得到维洛沙嗪盐酸盐。结果与结论经过3步反应合成目标化合物维洛沙嗪,总收率为28.4%。此外,还分离纯化得到两个盐酸维洛沙嗪的有关物质。目标化合物的结构均经1H-NMR和MS谱确证。 相似文献
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目的研究盐酸依福地平的合成工艺。方法以苯胺为原料,经4步反应制得中间体3-氨基-2-丁烯酸-2-(N-苄基N-苯基)-氨基乙酯(5);以新戊二醇和间硝基苯甲醛为原料,经过4步反应制得中间体3-(5,5-二甲基-2-氧代-2-[1,3,2]二氧杂磷杂环己基)-4-(3-硝基苯基)-丁-3-烯-2-酮(9);中间体5和9经环合、成盐反应制得盐酸依福地平。结果与结论目标化合物的结构经IR、MS和。H-NMR谱确证。改进后的工艺路线操作简便。总收率达39.5%,适合工业化生产。 相似文献
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目的合成抗哮喘药盐酸川丁特罗。方法以2-三氟甲基苯胺为起始原料,经碘代、酰化、取代、Stephen还原、水解、氯代、Wittig反应、环氧化、胺化和成盐10步反应制得盐酸川丁特罗。结果与结论目标化合物的总收率为5.71%,其结构经质谱、1H-NMR谱确证。改进后的合成工艺缩短了步骤、简化了操作、降低了合成成本,适合工业化生产。 相似文献
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《中国药物化学杂志》2015,(6):446-449
目的为了加强对α受体阻滞剂类抗高血压药盐酸特拉唑嗪原料药的质量控制,合成了盐酸特拉唑嗪的3个特定杂质。方法以盐酸特拉唑嗪为原料,经重氮化、水解反应制得1-(4-羟基-6,7-二甲氧基-2-喹唑啉基)-4-[(四氢呋喃基)碳酰基]-哌嗪(杂质B);以盐酸特拉唑嗪为起始原料,经水解制得1-(4-氨基-6,7-二甲氧基-2-喹唑啉基)哌嗪二盐酸盐(杂质C);以2-氯-4-氨基-6,7-二甲氧基喹唑啉为起始原料,经N-取代反应制得1,4-二(4-氨基-6,7-二甲氧基-2-喹唑啉基)哌嗪二盐酸盐(杂质E)。结果与结论合成的3种杂质的结构经1H-NMR、MS确证,纯度相当或优于美国药典杂质对照品,可以作为盐酸特拉唑嗪原料药质量控制的杂质对照品。 相似文献
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目的建立革除汞盐的非水电位滴定法测定盐酸莫雷西嗪原料的含量。方法建立以冰醋酸与醋酐(1:3)为溶剂的高氯酸非水电位滴定法测定盐酸莫雷西嗪原料的含量。结果与2005年版《中国药典(二部)》方法测定结果一致。结论该法操作简单,灵敏度高,准确可靠,重复性及稳定性良好,适于盐酸莫雷西嗪原料的含量测定。 相似文献
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目的合成雷诺嗪并进行工艺改进。方法以2,6-二甲基苯胺、愈创木酚为原料,经酰化、烃化等4步反应制得雷诺嗪。结果总收率36.8%,产物结构经熔点、红外光谱和核磁共振确证。结论此合成路线操作简单可行、适合工业化生产。 相似文献
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目的 :合成盐酸川丁特罗的重要中间体3-氯-4-氨基-5-三氟甲基苯乙酮。方法: 以邻-三氟甲基苯胺为起始原料,经碘代、酰化、氰基取代、水解、取代、氯代和烃化7步反应得到盐酸川丁特罗的重要中间体。结果与讨论: 目标化合物的结构经1H-NMR和MS确证,总收率为8.9 %。该合成工艺操作简便,适合工业化生产。 相似文献
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[目的] 探讨3,4-二甲氧基苄胺的合成方法。[方法] 设计两条合成路线:路线Ⅰ,以香兰素为原料,经甲基化、肟化及铝镍合金还原得目标物;路线Ⅱ,以3,4-二甲氧基苯甲酸为原料,经氯化、氨解及还原得目标物。[结果]两种方法所合成的目标物结构经FSI( )MS、1HNMR得以确证;路线I总收率为81.7%,路线I总收率为55.6%。 相似文献
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目的 合成3个重要的药物中间体。方法 以乳酸乙酯、卤代烷为起始原料,通过烷基化、格氏化、还原、胺解、成盐5步反应得到目标化合物。结果与结论 合成目标化合物2-甲氧基-3-戊胺盐酸盐(1)、2-乙氧基-3-戊胺盐酸盐(2)和2-乙氧基-N-甲基-3-戊胺盐酸盐(3),收率分别为18.1%、18.8%、14.3%。目标化合物的结构经MS和1H-NMR谱确证。 相似文献
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顶空毛细管气相色谱法测定盐酸莫雷西嗪中残留溶剂的含量 总被引:1,自引:1,他引:0
目的建立顶空气相色谱法测定盐酸莫雷西嗪中甲醇、乙醇、异丙醇、二氯甲烷、乙酸乙酯、四氢呋喃、甲苯7种有机溶剂残留量的方法。方法色谱柱为DB-624石英毛细管柱,柱温采用程序升温,检测器为FID检测器,检测器温度为250℃,进样口温度为150℃,以水为溶解介质。结果甲醇、乙醇、异丙醇、二氯甲烷、乙酸乙酯、四氢呋喃、甲苯的质量浓度的线性范围分别为12.0~240 mg.L-1(r=1.000 0)、10.0~200 mg.L-1(r=0.999 9)、10.0~200 mg.L-1(r=0.999 9)、1.20~24 mg.L-1(r=0.999 9)、10.0~200 mg.L-1(r=0.999 9)、1.44~28.8 mg.L-1(r=0.999 8)、1.78~35.6 mg.L-1(r=0.999 7);平均回收率为98.1%~99.5%(RSD=0.6%~1.7%);定量限为0.22~11.91 mg.L-1;3批样品中7种有机溶剂残留量均符合《中华人民共和国药典》要求。结论本方法简单、准确、灵敏度高、重现性好,可用于该药物中有机溶剂残留量的测定。 相似文献
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D. L. Howrie H. J. Pieniaszek Jr. R. N. Fogoros R. P. Juhl W. L. Schary C. C. Whitney Jr. L. W. Dittert 《European journal of clinical pharmacology》1987,32(6):607-610
Summary Moracizine (ethmozine) is a phenothiazine derivative with demonstrated antiarrhythmic activity. To characterize the pharmacokinetics
and material balance relationships in humans, we have given14C-moracizine·HCl as a single oral dose of 500 mg (50 μCi) to six healthy men. Plasma, urine, and faecal samples were collected
for 7 days after administration and the concentrations of total radioactivity and intact moracizine were determined by liquid
scintillation counting and HPLC, respectively.
Urine and faecal recovery accounted for 95% of the administered radioactivity. Most of this radioactivity was found in the
faeces (59%). Only 0.05% of the dose was recovered from urine as intact moracizine.
The Cmax and AUC for moracizine equivalents of total radioactivity were 4- and 18-fold higher, respectively, than the corresponding
values for intact moracizine. Additionally, both the disappearance of total radioactivity from plasma and its excretion rate
into urine were slower in comparison to intact drug. Terminal t1/2 values calculated from plasma concentration-time data were 85.2 and 3.5 h for total radioactivity and intact moracizine,
respectively. However, based on urinary excretion rates, the t1/2 for total radioactivity was shorter (29.3 h) while the t1/2 for intact drug was comparable (2.7 h) to the results obtained from the plasma data. The oral plasma clearance of moracizine
was relatively large (2.2l·min−1), suggesting first-pass metabolism. The estimated oral systemic availability of moracizine was 34%. 相似文献
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范石虎 《中国药物化学杂志》2013,23(4):295-296
目的改进盐酸沙格雷酯的合成工艺。方法以2-[2-(3-甲氧基苯基)乙基]苯酚为起始原料,经成醚反应、胺解反应、酯化成盐得盐酸沙格雷酯。结果目标产物的结构经元素分析、IR、1H-NMR谱数据确证,且质量符合日本药典标准。结论改进后的工艺操作简便、产品质量稳定、收率高、成本低,更适合工业化生产。 相似文献
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W J Bodell 《Chemical research in toxicology》1999,12(10):965-970
The purpose of this study was to examine the influence of cations on the formation of the individual DNA alkylation products derived from 1-(2-chloroethyl)-1-nitrosourea (CNU). Reaction of calf-thymus DNA with [(3)H]CNU in 10 mM triethanolamine buffer produced 13 DNA adducts. Seven of these adducts were identified as N7-(2-hydroxyethyl)guanine, N7-(2-chloroethyl)guanine, 1, 2-(diguan-7-yl)ethane, N1-(2-hydroxyethyl)-2-deoxyguanosine, 1-(N1-2-deoxyguanosinyl)-2-(N3-2-deoxycytidyl)ethane, O(6)-(2-hydroxyethyl)-2-deoxyguanosine, and phosphotriesters. The ratios of the individual products indicated that the chloroethyl and hydroxyethyl adducts are derived from different alkylating intermediates. The influence of cations on the formation of these DNA alkylation products was investigated by the addition of either NaCl, MgCl(2), or spermine. The results demonstrated that (1) the levels of DNA alkylation were inversely proportional to ionic strength, (2) the extent of inhibition was dependent on the alkylation product, and (3) the order of relative effectiveness of inhibition of DNA alkylation by these cations was as follows: spermine > Mg > Na. These results support a model whereby reactions which proceed via an S(N)2 mechanism are more sensitive to the effects of ionic strength than reactions which proceed via an S(N)1 mechanism. In 9L cells treated with CNU, the same alkylation products were formed as in purified DNA; however, the product distribution was different. We interpret this to indicate that within cells, cations modify the reaction of intermediates derived from CNU with DNA. 相似文献