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1.
毛泽伟  张梦迪  饶高雄 《合成化学》2015,23(10):938-940
以3-羟基氮杂环丁烷盐酸盐为原料,与4-氟苯乙酮反应制得1-(4-乙酰苯基)-3-羟基氮杂环丁烷(1); 1经甲磺酰化反应、取代反应、还原反应及酰化反应,合成了6个新型的3-氨基氮杂环丁烷衍生物,其结构经1H NMR和13C NMR表征。  相似文献   

2.
以2,4-二羟基苯乙酮为原料,经4步反应合成了水黄皮籽素,总收率26%,其结构经1H NMR和HR-MS(ESI)确证。  相似文献   

3.
以对羟基苯甲醛和2,4-二羟基苯乙酮为起始原料,经过甲氧甲基化、溴代、Ullmann反应、羟醛缩合和脱保护等反应,完成了天然产物双查尔酮Luxenchalcone的全合成,关键步骤为Ullmann反应,重要中间体和目标产物的化学结构经 1H NMR,13C NMR和ESI-MS等表征确认.  相似文献   

4.
以苯甲醛和2,4,6-三羟基苯乙酮一水合物为起始原料,经C-异戊烯基化、氧化环化、碘甲烷保护羟基、羟醛缩合反应以及催化关环等步骤,以7.2%和5.7%的总收率实现了两个天然吡喃类黄酮obovatachalcone和(±)obovatin methyl ether的全合成,其结构经1H NMR, 13C NMR, IR和HR-MS(ESI)确证。  相似文献   

5.
以季铵盐为催化剂,由α-溴代苯乙酮合成α-羰酰氧基苯乙酮,然后在碱性条件下,高效制备了α-羟基苯乙酮,转化率和选择性分别为100.0%和91.2%,其结构经1H NMR确证。   相似文献   

6.
以2,4-二羟基苯乙酮和对羟基苯甲醛为原料,分别在3种催化条件(A: SOCl2/EtOH, B: KF/Al2O3配合超声,C: KOH/Al2O3配合微波固相反应)下合成了查尔酮类化合物异甘草素(3),其结构经1H NMR, 13C NMR和MS(ESI)确证。研究了3种催化条件下反应时间(A~C)和功率(B, C)对3产率的影响。结果表明:C为合成3的最优催化方法(于150 W反应0.03 h,产率93.5%)。  相似文献   

7.
孟令国  杨明明 《合成化学》2011,19(6):796-798
以邻羟基苯乙酮衍生物为原料,经溴化反应和叠氮化反应合成了一系列邻羟基α-叠氮苯乙酮衍生物,其结构经1H NMR,13C NMR,IR及HR-MS表征.  相似文献   

8.
樊宏宇  张羽 《合成化学》2017,25(11):948-952
以1,3-二羟基苯和对羟基苯甲醛为起始原料,经赫氏酰化、羟基保护、克莱森 斯密特缩合及催化氢化反应首次合成天然产物去甲基构树宁B,总收率40.9%,其结构经1H NMR, 13C NMR和HR-MS(ESI TOF)确证。  相似文献   

9.
以4-二甲氨基苯甲醛和2-溴-4′-氟苯乙酮为原料,经缩合和取代反应制得4-二甲氨基-4′-(1-哌嗪基)查尔酮(2); 2与卤代烃反应合成了6个新型的查尔酮哌嗪衍生物,收率71%~88%,其结构经1H NMR,13C NMR和HR-MS表征。  相似文献   

10.
安敏  王伟  门靖 《合成化学》2019,27(1):61-64
以3-氨基-2-羟基-苯乙酮为起始原料,经酰胺化、缩合、环合及脱保护反应合成了普仑司特关键中间体8-氨基-4-氧代-2-(1H-四唑-5-基)-4H-1-苯并吡喃,总收率40.1%,其结构经1H NMR和MS确证。该路线中脱保护和环合两步反应采用了一锅法,并对合成工艺进行了优化。  相似文献   

11.
利用手持技术改进测定乙醇分子结构实验   总被引:1,自引:0,他引:1  
利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。  相似文献   

12.
13.
The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.  相似文献   

14.
实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。  相似文献   

15.
16.
非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。  相似文献   

17.
Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.  相似文献   

18.
由于石化行业的生产需要,其材质的使用具有多样性和广泛性,经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识,根据光谱仪的测试能力及标样的采集,实现了一个或几个元素测量范围的扩展,并对其测量的影响因素进行了研究。  相似文献   

19.
The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.  相似文献   

20.
The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.  相似文献   

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