安宫黄体酮母液中两个新化合物的分离与结构鉴定

目的研究药物安宫黄体酮中所含的杂质。方法应用柱色谱方法进行分离和纯化，NMR和MS等波谱方法确定结构。结果从安宫黄体酮母液中分离得到2个化合物。结论化合物1和2为新差向异构体，其结构分别鉴定为：17α-氧乙酰基-2β，6α-二甲基孕甾-4-烯-3，20-二酮；17α-氧乙酰基-2α，6α-二甲基孕甾-4-烯-3，20-二酮。     

米非司酮母液中杂质的分离和结构鉴定

目的: 研究药物米非司酮中的杂质。方法: 运用硅胶柱层析和半制备高效液相进行分离和纯化,其结构通过NMR和HREIMS等技术进行鉴定。结果: 从母液中分离得到3个化合物,其结构分别鉴定为17β-羟基-17α-(1-丙炔基)-雌甾-5, 9-二烯-3-酮环缩乙二醇(Ⅰ),11-[4-(二甲基氨基)苯基]-17β-羟基-17α-(1-丙炔基)-雌甾-5, 9-二烯-3-酮环缩乙二醇(Ⅱ),11-[4-(二甲基氨基)苯基]-17β-羟基-17α-(1-丙炔基)-雌甾-4, 10, 11-三烯-3-酮(Ⅲ)。结论: 3个杂质均为首次从药物米非司酮中确定,其中Ⅱ为新化合物。     

19-羟基雄甾-4-烯-3,17-二酮4-取代物的合成及其对睾丸素A环芳香化酶的抑制活性

以19-羟基雄甾-4-烯-3,17-二酮(1)为先导物,经4β,5β-环氧化得8,然后4-位,引入取代基如羟基、氯、溴及乙酰硫基(2、3、4及5)。并用HPLC法测定其对人胎盘微粒体睾丸素A环芳香化酶的相对抑制活性,结果表明3活性较强。     

天女木兰叶中甾类化合物的分离与鉴定

目的对天女木兰叶的化学成分进行分离和结构鉴定。方法采用硅胶、凝胶柱色谱和重结晶等分离方法对天女木兰叶的体积分数为90%的乙醇溶液提取物进行成分分离;通过谱学分析方法结合化合物理化性质对分离得到的化合物进行结构鉴定。结果分离得到8个化合物,分别鉴定为豆甾-4-烯-3,6-二酮(stigmast-4-en-3,6-dione,1),豆甾-4-烯-3β,6β-二醇(stigmast-4-en-3β,6β-diol,2),5α,8α-过氧-(22E,24R)-麦角甾-6,22-二烯-3β-醇[5α,8α-epidioxy-(22E,24R)-ergosta-6,22-dien-3β-ol,3],豆甾-4-烯-6β-羟基-3-酮(stigmast-4-en-6β-ol-3-one,4),β-谷甾醇(β-sitosterol,5),(22E,24R)-麦角甾-7,22-二烯-3β,5α,6β-三醇[(22E,24R)-ergosta-7,22-dien-3β,5α,6β-triol,6],豆甾-5-烯-3β,7α-二醇(stigmast-5-en-3β,7α-diol,7),胡萝卜苷(daucosterol,8)。结论化合物2-4、6、7为首次从木兰属植物中分离得到,化合物1为首次从该植物中分离得到。     

11β，17α-二羟基-17-丙酰基-1，4-雄甾二烯-3-酮的合成

目的 制备17-丙酰基功能化的甾体化合物11β,17α-二羟基-17-丙酰基-1,4-雄甾二烯-3-酮.方法 以泼尼松龙为原料,经5步反应合成目标物.结果 和结论 总收率为67.4%,通过NMR、MS等确证了中间体和目标物的结构.     

3-酮基-4-雄甾烯-17β-羧酸甲酯的合成改进

孕烯醇酮乙酸酯经溴仿反应、酯化、沃氏氧化得到非那雄胺的关键中间体3-酮基-4-雄甾烯-17β-羧酸甲酯,其中沃氏氧化用邻硝基苯甲醛为氧化剂,使用催化量异丙醇铝在甲苯中于95℃反应2h即可完成,收率85%.总收率71%.     

仙人掌中一个新α-吡喃酮成分的分离与结构鉴定

目的研究仙人掌的化学成分。方法应用多种柱色谱方法进行分离和纯化，NMR和MS等波谱解析化学结构。结果从仙人掌肉质茎的乙醇提取物中分离出6个化合物，其结构分别鉴定为：3-O-甲基异鼠李黄素(1)、4-乙氧基-6-羟甲基-α-吡喃酮(2)、正十七醇(3)、香草酸(4)、异鼠李黄素-3-O-鼠李糖苷(5)和芦丁(6)。结论化合物2为新化合物,化合物1、3、4、5均为首次从本属植物中分离得到，化合物6为本植物首次分离得到。     

快速分析测定大豆甾醇侧链降解底物的方法

建立了快速分析测定大豆甾醇侧链降解过程中底物大豆甾醇和产物雄甾-4-烯-3，17-二酮(AD)及雄甾-1，4-二烯-3，17-二酮(ADD)的方法。采用薄板层析(TLC)，在板层为硅胶60GF254，流动相为石油醚-乙酸乙酯(6：4)的条件下，成功的分离了底物与产物，从而能快速简便的监测底物的消耗与产物的生成情况。另外根据底物与产物AD与ADD在紫外区的吸收情况，利用254nm与298nm双波长测定ADD与AD的生成量。上述两种方法便于工厂对生产情况的同步检测。     

7α和7β-甲基-10β,17β-二乙酰氧基-4-雌甾烯-3-酮的合成

由于7α-甲基或10β-乙酰氧基4(5)烯-3-酮雌(雄)甾化合物具有显著的抗着床或抗蜕膜活性,我们合成了既具有7α-甲基或7β-甲基又具有10β-乙酰氧基的两个新甾族化合物(1_a)和(1_b)。经药理试验表明(1_a)和(1_b)对孕鼠均有抗早孕作用。     

仙人掌中一个新α-吡喃酮成分的分离与结构鉴定

目的　研究仙人掌的化学成分。方法　应用多种柱色谱方法进行分离和纯化 ,NMR和MS等波谱解析化学结构。结果　从仙人掌肉质茎的乙醇提取物中分离出 6个化合物 ,其结构分别鉴定为 :3 O 甲基异鼠李黄素 (1)、4 乙氧基 6 羟甲基 α 吡喃酮 (2 )、正十七醇 (3)、香草酸 (4)、异鼠李黄素 3 O 鼠李糖苷 (5 )和芦丁 (6 )。结论　化合物2为新化合物 ,化合物 1、3、4、5均为首次从本属植物中分离得到 ,化合物 6为本植物首次分离得到。     

ent-Kaurenoids from the roots of Cacalia pilgeriana

Two new ent-kaurenoids,19-acetoxyl-ent-3β,17-dihydroxykaur-15-ene (1), 19-acetoxyl-ent-3β-hydroxykaur-15-en-17-al (2), together with seven known ent-kaurenoids: ent-kaur-16-en-19-al (3), ent-kaur-16-en-19-oic acid (4), ent-kauran-16β,17-diol (5), ent-15β, 16β-epoxy-17-hydroxykauran-19-oic acid (6),19-acetyl-ent-3β-hydroxyl-kaur-16-ene (7), ent-3β,19-dihydroxykaur-16-ene (8), ent-17-hydroxykaur-15-ene (9), were isolated from Cacalia pilgeriana. Their structures were elucidated by spectroscopic methods including 2D NMR spectral analysis.     

A New d-Lactone Containing Triterpene from the Flowers of Calendula officinalis

A new δ-lactone containing triterpene, 4β-methylcholest-20-en-12a-ol-3β-olide, was isolated from Calendula officinalis Linn. flowers in addition to three known compounds, lanast-20(22)-en-3β-ol, stigmast-5,22-dien-3β-ol, and stigmast-5,24(28)-dien-3β-ol. Their structures were elucidated by spectroscopic (UV, IR, NMR, and MS) methods and chemical reactions.     

Steroids from Harrisonia abyssinica

In addition to the known sterols and ketosteroids beta-sitosterol (24 alpha-ethylcholest-5-en-3 beta-ol), stigmasterol (24 alpha-ethylcholesta-5,22-dien-3 beta-ol), campesterol (24 alpha-methylcholest-5-en-3 beta-ol), beta-sitostenone (stigmast-4-en-3-one, 24 alpha-ethylcholest-4-en-3-one), stigmastenone (stigmasta-4,22-dien-3-one, 24 alpha-ethylcholesta-4,22-dien-3-one), campestenone (24 alpha-methylcholest-4-en-3-one), and stigmasta-3,5-dien-7-one (24 alpha-ethylcholesta-3,5-dien-7-one), the new steroids stigmasta-3,5,22-trien-7-one (24 alpha-ethylcholesta-3,5,22-trien-7-one), and campesta-3,5-dien-7-one (24 alpha-methylcholesta-3,5-dien-7-one) were isolated from the stem bark of Harrisonia abyssinica and identified by NMR and mass spectrometry.     

An efficient semi-synthesis of 1-hydroxyl oleanolic acid analogs

An efficient route for the semi-synthesis of either 1α- or 1β-OH epimers of 1-hydroxy-3-deoxyolean-12-en-28-oic acid (1), 6–8 steps from oleanolic acid is reported. The synthesis involves stereoselective formation of α,β-unsaturated epoxy ketone and subsequent Wharton reaction as key steps, offering a new access to the 1-O-substituted oleanolic acid-type pentacyclic triterpenoids.     

苦葛蔓中的新三萜成分

目的： 对苦葛蔓(Pueraria peduncularis Grah.)酸水解产物中的化学成分进行分离和结构鉴定。方法： 用各种色谱技术进行分离,得到3个五环三萜化合物,用MS,¹HNMR,¹³CNMR(DEPT),HMQC,HMBC和NOESY谱鉴定化合物。结果： 经光谱鉴定化合物1为3β,15α,23-三羟基齐墩果-12-烯-16-酮,化合物2为3β,15α-二羟基齐墩果-12-烯-16-酮,化合物3为3β,22β,24-三羟基齐墩果-12-烯(soyasapogenol B)。结论： 化合物1和化合物2为新化合物。     

Trypanosomicidal kaurane diterpenes from Wedelia paludosa

The diterpenes ent-kaur-16-en-19-oic acid, ent-kaur-9(11),16(17)-dien-19-oic acid and 3 alpha-angeloiloxy-ent-kaur-16-en-19-oic acid were identified as trypanosomicidal compounds of the ethanolic extract from the aerial parts of Wedelia paludosa D.C. (Asteraceae), showing activity up to the lowest dose of 0.68 mg/mL in the in vitro assay against trypomastigotes of T. cruzi, the causative agent of Chagas' disease (American trypanosomiasis). The other isolates, friedelan-3 beta-ol, ent-kaur-16 alpha-ol-19-oic acid, beta-amyrin acetate and (22-E)-stigmasta-5,22-dien-3 beta-ol, were inactive. This is the first report on the trypanosomicidal activity of ent-kaur-9(11),16(17)-dien-19-oic acid and 3 alpha-angeloiloxy-ent-kaur-16-en-19-oic acids; this effect was already known for ent-kaur-16-en-19-oic acid.     

Two new phenol derivatives from Stereum hirsutum FP-91666

Two new phenol derivatives, 2-(3-methyl-2-buten-1-yl)-4-methoxyethyl-phenol (1) and 5-hydroxy-4-(hydroxymethyl)-2-(3-methylbut-2-en-1-yl)cyclohex-4-en-1-one (2), together with eight known compounds consisting of phenol derivatives (3 and 4), niacinamide (5), and five ergosta type compounds (6–10), were isolated from solid fermentation products of Stereum hirsutum FP-91666. Two new structures were elucidated by extensive spectroscopic methods, including 1D NMR and 2D NMR, and HR-EI-MS experiments.     

Bioactive triterpenoids from the stem bark of Picea glehni

Two new triterpenoids, 3 alpha-methoxyserrat-14-en-21 beta-yl formate (1), and 24-methylcycloartenone (2), were isolated from the stem bark of Picea glehni (Fr. Schm.) Masters together with three known triterpenoids, 3 alpha-methoxyserrat-14-en-21 beta-ol, 3 beta-methoxyserrat-14-en-21 beta-ol, and piceanonol A. Compounds 1, 2, and a synthetic sample, 3 alpha-methoxyserrat-13-en-21 beta-yl formate showed potent inhibitory effects on Epstein-Barr virus early antigen (EBV-EA) activation induced by the tumor promoter 12-O-tetradecanoylphorbol-13-acetate (TPA).     

New pentacyclic triterpenes from the roots of Hemidesmus indicus

Phytochemical studies on the roots of Hemidesmus indicus resulted in the isolation of six new pentacyclic triterpenes including two oleanenes identified as olean-12-en-21 beta-yl acetate, and olean-12-en-3 alpha-yl acetate, three ursenes characterized as 16(17)-seco-urs-12,20(30)-dien-18 alpha H-3 beta-yl actetate, urs-20(30)-en-18 beta H-3 beta-yl acetate and 16(17)-seco-urs-12,20(30) dien-18-alpha H-3 beta-ol and a lupene formulated us lup-1,12-dien-3-on-21-ol including a known compound, beta-amyrin acetate, on the basis of spectroscopic techniques and chemical means.