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Effect of Temperature on the Reaction of 2-(N-acetylamine)-3-(3,5-di-<i>tert</i>-butyl-4-hydroxyphenyl)-propionic Acid with Oxygen in an Alkaline Condition
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作者 A. A. Volodkin G. E. Zaikov +3 位作者 L. N. Kurkovskaja S. M. Lomakin I. M. Levina E. V. Koverzanova 《Advances in Chemical Engineering and Science》 2015年第3期262-269,共8页
Results of oxidation 2-(N-acetylamine)-3-(3,5-di-tert-butyl-4-hydroxyphenyl)-propionic acid oxygen depend on temperature. At 55℃?- 60℃, 2,4-di-tert-butylbicyclo(4,3,1)deca-4,6-dien-8-(N-acetylamine)-3,9-dion-1-oxa i... Results of oxidation 2-(N-acetylamine)-3-(3,5-di-tert-butyl-4-hydroxyphenyl)-propionic acid oxygen depend on temperature. At 55℃?- 60℃, 2,4-di-tert-butylbicyclo(4,3,1)deca-4,6-dien-8-(N-acetylamine)-3,9-dion-1-oxa is formed. The constitution is based on dates of spectrums 1Н and 13С NMR. At 95℃?- 97℃, mixtures of 2,4-di-tert-butylbicyclo(4,3,1)deca-4,6-dien-8-(N-acetylamine)-3,9-dion-1-oxa and of 6,8-di-tert-butyl-3-(N-acetylamine)spiro(4,5)deca-1-oxa-5,8-dien-2,7-dione are produced. Structures are calculated by the method of Hartrii-Foka. Values of enthalpies and of entropies allow to assume dynamic isomerism. 展开更多
关键词 2-(N-acetylamine)-3-(3 5-di-tert-butyl-4-hydroxyphenyl)-propionic Acid 6 8-di-tert-butyl-3-(N-acetylamine)spiro(4 5)deca-1-oxa-5 8-dien-2 7-dione Oxidation by OXYGEN 2 4-Di-tert-butylbicyclo(4 3 1)deca-4 6-dien-8-(N-acetylamine)-3 9-dion-1-oxa NMR-Spectroscopy
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A New Halogenated Biindole and A New Apo-carotenone from Green Alga Chaetomorpha basiretorsa Setchell 被引量:6
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作者 DaYongSHI LiJunHAN +5 位作者 JieSUN ShuaiLI SuJuanWANG YongChunYANG XiaoFAN JianGongSHI 《Chinese Chemical Letters》 SCIE CAS CSCD 2005年第6期777-780,共4页
A new halogenated biindole and a new apo-carotenone have been isolated from the ethanolic extract of the green alga Chaetomorpha basiretorsa Sethcell. On the basis of chemical and spectroscopic methods including 2D NM... A new halogenated biindole and a new apo-carotenone have been isolated from the ethanolic extract of the green alga Chaetomorpha basiretorsa Sethcell. On the basis of chemical and spectroscopic methods including 2D NMR technique, their structures have been elucidated as 4,4′-dichloro-5,5′-dibromo-7,7′-dimethoxy-2,2′-bi-1H-indole and 1′S*,4′R*-8-(4′-hydroxy-2′,6′,6′- trimethylcyclohex-2-enyl)-6-methyloct-3E,5E,7E-trien-2-one, respectively. 展开更多
关键词 Green alga Chaetomorpha basiretorsa Sethcell 4 4-dichloro-5 5′-dibromo-7 7′-di- methoxy-2 2′-bi-1H-indole 1′S* 4′R*-8-(4-hydroxy-2′ 6′ 6′-trimethylcyclohex-2-enyl)-6-methyl- oct-3E 5E 7E-trien-2-one.
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苏木心材中一个新黄酮类化合物 被引量:2
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作者 舒诗会 韩景兰 +1 位作者 杜冠华 秦海林 《中国中药杂志》 CAS CSCD 北大核心 2008年第8期903-905,共3页
目的:从苏木Caesalpinia sappan中寻找新的活性成分。方法:用溶剂萃取及硅胶正相色谱进行活性成分的分离纯化,根据理化性质、光谱数据进行结构鉴定。结果:从苏木95%乙醇提取物中分离得到了9个化合物:3,8-dihydroxy-4,10-dimethoxy-7-oxo... 目的:从苏木Caesalpinia sappan中寻找新的活性成分。方法:用溶剂萃取及硅胶正相色谱进行活性成分的分离纯化,根据理化性质、光谱数据进行结构鉴定。结果:从苏木95%乙醇提取物中分离得到了9个化合物:3,8-dihydroxy-4,10-dimethoxy-7-oxo-[2]benzopyrano[4,3-b][1]benzopyran-7-(5H)-one(1),3-deoxysappanchal-cone(2),sappanchalcone(3),3-deoxysappanone B(4),鼠李素(rhamnetin,5),原苏木素C(protosappanin C,6),3,7-di-hydroxy-chroman-4-one(7),己二酸二甲酯(8),胡萝卜苷(daucosterin,9)。结论:化合物1为新化合物,化合物7,8为首次从该植物中分离得到。药理筛选结果表明,化合物3对多种癌细胞株具有一定的抑制活性。 展开更多
关键词 苏木 黄酮 3 8-dihydroxy-4 benzopyrano[4 benzopyran-7-(5H)-one 细胞毒活性
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Chemical Constituents of One Species of Endophytic Fungus in Taxus chinensis 被引量:3
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作者 张集慧 郭顺星 +1 位作者 杨峻山 肖培根 《Acta Botanica Sinica》 CSCD 2002年第10期1239-1242,共4页
Three compounds were obtained from the mycelia of an endophytic fungus Gliocladium sp. (designated as strain F) of Taxus chinensis (Pilg.) Rehd. growing in Fujian Province, China. Their structures were determined on t... Three compounds were obtained from the mycelia of an endophytic fungus Gliocladium sp. (designated as strain F) of Taxus chinensis (Pilg.) Rehd. growing in Fujian Province, China. Their structures were determined on the basis of spectral analysis. (20S,22S)-4a-homo-22-hydroxy-4-oxaergosta-7,24(28)-dien-3-one was a novel compound. 4,8,12,16-tetramethyl-1,5,9,13-tetraoxacyclohexadecane-2,6,10,14-tetraone was firstly isolated from the genus ofGliocladium and 6,9-epoxyergosta-7,22-dien-3-ol was firstly obtained from the strain F. 展开更多
关键词 Taxus chinensis (20S 22S)-4a-homo-22-hydroxy-4-oxaergosta-7 24 (28)-dien-3-one chemical constituent Gliocladium sp.
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UPLC-Q/TOF法同时定性定量分析滇芹药材中主要化学成分 被引量:8
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作者 秦伟瀚 冉继春 +4 位作者 叶良红 花雷 王云红 郭延垒 阳勇 《中草药》 CAS CSCD 北大核心 2018年第15期3576-3582,共7页
目的建立UPLC-Q/TOF法同时定性、定量分析滇芹中主要化学成分。方法采用超高效液相色谱串联飞行时间质谱法进行分析,色谱柱为Agilent Poroshell 120 Hilic,流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,体积流量0.3 m L/min;定性、定量采用Q-... 目的建立UPLC-Q/TOF法同时定性、定量分析滇芹中主要化学成分。方法采用超高效液相色谱串联飞行时间质谱法进行分析,色谱柱为Agilent Poroshell 120 Hilic,流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,体积流量0.3 m L/min;定性、定量采用Q-TOF正负离子全扫描+IDA(信息关联采集)模式。结果利用已建立的筛查数据库将满足质量误差小于5×10-6、同位素分布正确且含有二级碎片的离子作为分析目标化合物,结合软件Formula Finder、Mass Calculators等功能、在线数据库(Human Metabolome Database、Pub Chem、Chemical Book等)及二级碎片裂解规律,共鉴定出23个化合物,滇芹首次发现4个化合物。确定阿魏酸为定量分析指标性成分,其定量、定性离子分别为178和149;阿魏酸检测质量浓度线性范围为1.14~1 140 ng/m L(r=1.000),检测限、定量限分别为0.87、2.91 ng/m L,精密度、稳定性、重复性试验的RSD<2%,加样回收率为98.13%~101.25%(RSD=1.37%,n=5)。结论该方法灵敏度高、重现性好,分析快速、准确、可靠,可用于同时定性、定量检测滇芹药材中主要化学成分;云南滇芹中阿魏酸含量要高于西藏滇芹。 展开更多
关键词 滇芹 UPLC-Q/TOF 阿魏酸 6-(2-methoxyvinyl)-7-methyl-2H-1-benzopyran-2-one 1-O-β-D-glucopyranosyl-1 3-octanediol 2-pentylbutanedioic acid 4 4-dimethylcholesta-8(9) 14-dien-3β-ol
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A stereoselective formal synthesis of (±)-Prelog-Djerassi lactonic acid
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作者 LIU, Zhi-Yu MA, Jing-YuanShanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 354 Fenglin Lu, Shanghai 200032, China 《Chinese Journal of Chemistry》 SCIE CAS CSCD 1995年第2期190-192,共3页
During the course of our program in the synthesis of natural products by retroDiels-Alder reaction using a rigid molecule tricyclo-[5.2.1.0]-deca-4,8-dien-3-one(1) as the starting material, it was observed that aldo... During the course of our program in the synthesis of natural products by retroDiels-Alder reaction using a rigid molecule tricyclo-[5.2.1.0]-deca-4,8-dien-3-one(1) as the starting material, it was observed that aldol condensation of compound (2) 展开更多
关键词 Prelog-Djerassi lactonic acid retro-Diels-Alder reaction tricyclodeca-4-8-dien-3-one.
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二妙丸HPLC指纹图谱及UPLC-LTQ-Orbitrap成分分析 被引量:7
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作者 雷蓉 周亚楠 +1 位作者 刘永利 冯丽 《中草药》 CAS CSCD 北大核心 2017年第17期3511-3516,共6页
目的建立二妙丸的HPLC指纹图谱质量评价方法,并对二妙丸中的化学成分进行UPLC-LTQ-Orbitrap定性分析。方法指纹图谱采用HPLC法,色谱柱为Shiseido C18柱(250 mm×4.6 mm,5μm),乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,体积流量为1.... 目的建立二妙丸的HPLC指纹图谱质量评价方法,并对二妙丸中的化学成分进行UPLC-LTQ-Orbitrap定性分析。方法指纹图谱采用HPLC法,色谱柱为Shiseido C18柱(250 mm×4.6 mm,5μm),乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,体积流量为1.0 m L/min,检测波长为330 nm,以黄柏、苍术混合对照药材生成的色谱图为标准对照图谱,采用"中国药典委员会相似度评价软件(2012A)"对样品进行相似度评价;采用UPLC-LTQ-Orbitrap技术对二妙丸中化学成分进行定性分析,色谱柱为Thermo Scientific Syncronis C18柱(100 mm×2.1 mm,1.9μm),乙腈-0.1%甲酸水溶液梯度洗脱,经DAD检测器后采用LTQ-Orbitrap Elite质谱正离子模式采集,各成分的一级全扫描离子在离子阱内进行CID多级质谱、FT检测高分辨质谱数据分析。结果所建立的指纹图谱有10个共有色谱峰,20批样品的相似度在0.869~0.992。通过对照品指认、文献比对以及高分辨质谱数据解析,鉴定了21个化学成分,分别为neo-chlorogenic acid、木兰箭毒碱、竹叶椒碱、木兰花碱、3-O-feruloylquinic acid、蝙蝠葛碱、demethyleneberberine、oxyberberine、非洲防己碱、药根碱、小檗红碱、巴马汀、小檗碱、丁香酸、咖啡酸、(E)-4-(3-hydroxyprop-1-en1yl)-2-methoxyphenol、白术内酯II、acetosyringone、白术内酯I、selina-4(14),7(11)-dien-8-one、苍术素。结论建立的二妙丸HPLC指纹图谱专属性强,重现性好,结合液质联用技术的定性分析,可全面评价二妙丸的内在质量。 展开更多
关键词 二妙丸 指纹图谱 HPLC UPLC LTQ-Orbitrap 质量评价 成分分析 相似度评价 neo-chlorogenic ACID 木兰箭毒碱 竹叶椒碱 木兰花碱 3-O-feruloylquinic ACID 蝙蝠葛碱 demethyleneberberine oxyberberine 非洲防己碱 药根碱 小檗红碱 巴马汀 小檗碱 丁香酸 咖啡酸 (E)-4-(3-hydroxyprop-1-en1yl)-2-methoxyphenol 白术内酯Ⅱ ACETOSYRINGONE 白术内酯Ⅰ selina-4(14) 7(11)-dien-8-one 苍术素
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Two new terpenoids from Reduning Injection 被引量:2
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作者 Hai-bo Li Biao Yang +6 位作者 Wen Ge Ze-yu Cao Liang Cao Yang Yu Zhen-zhong Wang Xin-sheng Yao Wei Xiao 《Chinese Herbal Medicines》 CAS 2020年第2期183-187,共5页
Objective:To study the antipyretic and anti-inflammatory constituents from the active fraction of Reduning(RDN)Injection.Methods:In this study,the active fraction of RDN Injection was screened by the LPS-induced mouse... Objective:To study the antipyretic and anti-inflammatory constituents from the active fraction of Reduning(RDN)Injection.Methods:In this study,the active fraction of RDN Injection was screened by the LPS-induced mouse endotoxin shock model.The chemical constituents were isolated by chromatography on HP-20 macroporous adsorptive resins,silica gel,ODS columns and reverse phase MPLC and HPLC repeatedly,and their structures were elucidated based on spectroscopic analysis(HR-ESI-MS,NMR,ECD)and chemical methods.Meanwhile,we evaluated the anti-inflammatory activities of the isolates by measuring their inhibitory effects on TNF-αproduction in LPS stimulated RAW 264.7 macrophages.Results:The 95%ethanol eluate of RDN Injection by the macroporous adsorption resin column was proved to be the antipyretic and anti-inflammatory active fraction of this injection.A novel iridoid,named jasminoide A(1),and a new guaiane sesquiterpenoid,named(1 R,7 R,8 S,10 R)-7,8,11-trihydroxy-4-guaien-3-one(2),were isolated from Reduning injection,and compound 2 can inhibit TNF-αproduction with IC50 values of 72.24μmol/L.Conclusion:In this study,two new terpenoids were isolated from Reduning Injection,and compound 2 showed inhibitory activity against LPS-activated TNF-αproduction in RAW 264.7 cells in vitro. 展开更多
关键词 (1R 7R 8S 10R)-7 8 11-trihydroxy-4-guaien-3-one ANTI-INFLAMMATION jasminoide A Reduning Injection TNF-Α
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