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吡啶氧基苯基哌嗪取代丙醇类α_1受体拮抗剂的合成
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作者 季红 黄碧云 袁牧 《中国医药导报》 CAS 2013年第27期106-107,共2页
目的设计合成具有α1受体拮抗活性的1-(吡啶-3-氧)-3-(4-苯基-1-哌嗪)-2-丙醇类化合物。方法在NaH存在下,3-羟基吡啶衍生物(1)和3-氯-1,2-环氧丙烷(2)在DMF中于60℃反应生成3-(吡啶-3-氧)-1,2-环氧丙烷(3),再经苯基哌嗪对环氧开环,合成... 目的设计合成具有α1受体拮抗活性的1-(吡啶-3-氧)-3-(4-苯基-1-哌嗪)-2-丙醇类化合物。方法在NaH存在下,3-羟基吡啶衍生物(1)和3-氯-1,2-环氧丙烷(2)在DMF中于60℃反应生成3-(吡啶-3-氧)-1,2-环氧丙烷(3),再经苯基哌嗪对环氧开环,合成了1-(吡啶-3-氧)-3-(4-苯基-1-哌嗪)-2-丙醇衍生物(4)。所合成的化合物经MS、1H-和13C-NMR谱确证其结构。结果采用两步反应合成了1-(吡啶-3-氧)-3-(4-苯基-1-哌嗪)-2-丙醇衍生物,这些化合物具有明显的α1受体拮抗活性。结论该合成方法适合于吡啶氧基苯基哌嗪取代丙醇类衍生物的合成,总收率达68%以上。 展开更多
关键词 吡啶-3-醇 1-(吡啶-3-氧)-3-(4-苯基-1-哌嗪)-2-丙 合成 α1 受体拮抗剂
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Synthesis and Solid Phase Extraction Performance Study of NNAL-specific Molecularly Imprinted Polymers Using Dummy Templates 被引量:2
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作者 张志丹 郑赛晶 +3 位作者 杨俊 王维妙 刘百战 朱晓兰 《Chinese Journal of Chemical Physics》 SCIE CAS CSCD 2013年第3期361-368,I0004,共9页
Dummy molecularly imprinted polymers (DMIPs) for 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) were produced using three structural analogues as dummy template molecules. The chosen analogues were 4-(a... Dummy molecularly imprinted polymers (DMIPs) for 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) were produced using three structural analogues as dummy template molecules. The chosen analogues were 4-(acetymethylamino)-1-(3-pyridyl)-butanol, 4- (methylamino)-1-(3-pyridyl)-1-butanol, and 1-(3-pyridyl)-1,4,-butanediol. The molecular recognition characteristics of the produced polymers were evaluated by X-ray photoelec- tron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FT-IR). Interactions between NNAL and methacrylic acid should be cooperative hydrogen bonds while the ni- trogen atom of the pyridine ring and the oxygen atom of the nitroso group in NNAL are two of the hydrogen-bond acceptors. It was further demonstrated that DMIP synthesized by 4-(acetymethylamino)-1-(3-pyridyl)-butanol had the best binding performance by XPS and FT-IR. Then dummy molecularly imprinted solid phase extraction (DMISPE) was developed for the determination of the analyte using the hit polymer as the sorbing material. Under optimal conditions, the recovery of NNAL dissolved in standard solution reached 93%. And the investigated polymer exhibited much higher binding of NNAL when nicotine was acted as the competitive molecule. Also the proposed method was applied to the measurement of NNAL spiked in blank urine samples with recoveries ranging from 87.2% to 101.2%. 展开更多
关键词 Molecularly imprinted polymer Dummy template 4-(Methylnitrosamino)-1-(3-pyridyl)-1-butanol Solid phase extraction
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