茶叶中咖啡因的提取实验装置的改进与探索

"茶叶中咖啡因的提取"是有机化学实验的一个经典实验,本文对该实验所用的原索氏提取器进行改进,得到内通气集热式索氏提取器并用于实验教学。通过对照实验,对改进索氏提取器和原索氏提取器的提取效果进行比较。结果表明,改进装置具有原装置的功能和特点,且提取时间更短、提取温度和提取率更高,可在高校推广使用。     

索氏提取器的简易替代装置

索氏提取器是化学实验中常用的提取装置,其特点是操作简单,具有连续性,提取率较高,但该装置造价高,虹吸管易破碎,装料及清理较困难。因此,我们对其进行了一些改进。     

咖啡因的升华装置的优化和形象化展现

“茶叶中咖啡因的提取实验”是有机化学的一个经典实验。对传统的升华装置进行了改进,让升华实验更加简单高效,并且能够看到咖啡因晶体聚集和长大的过程,该装置便于咖啡因的收集,能对所收集的咖啡因进行定量计算,同时增加了采用薄层色谱法对浓缩液中咖啡因进行定性鉴定的实验环节。改进的实验丰富了实验内容,降低了实验可能的失误,提高了实验的安全性,创造性地运用实验室的显微熔点仪和智能手机成功地对咖啡因晶体的形貌进行了拍摄,增加了实验的趣味性。     

Soxhlet提取器的简易替代装置

Ｓｏｘｈｌｅｔ提取器是化学实验室中常用的一种玻璃仪器 ,其特点是操作简单 ,具有连续性 ,提取效率较高 ,但该装置造价高 ,虹吸管容易破碎且清洗起来比较困难 ,在使用和保管中都需要十分小心。如我们在茶叶中提取咖啡碱的实验里 ,每次都是要求学生细心进行操作 ,尽管如此 ,由于Ｓｏｘｈｌｅｔ提取器的提抽虹吸管很细 ,每个学期经学生使用下来都要损坏一两套。更由于学校经费不足 ,不可能购买许多备用品 ,有时即使有钱也不能及时到货 ,使得实验过程中Ｓｏｘｈｌｅｔ提取器显得严重不足 ,为此我们利用现有的一些非磨口仪器 ,制作了简易的提取…     

一种用于从固体中提取溶质的热提取装置

一种用于从固体中提取溶质的热提取装置王杰，任仲皎，伍明（中南民族学院化学系，武汉４３００７４）在化学合成和天然产物的提取中，传统的方法一般是利用索氏或梯氏提取器来提取溶质，也可用容器直接浸提溶质￣［１］。上述方法一般均需将固体磨成微细颗粒，且提取效率...     

一种快速抽提微量成分的热逆流提取装置

液固萃取在化学实验及研究中常常遇到,索氏提取器是液团萃取普遍采用的装置,它具有简单、提取率高等特点,但采用索氏提取器从较大体积的固体样品中提取微量成分是很困难的。对于要求在较高温度下进行液固萃取也难于实现。为此我们设计了一种热逆流提取器,它不仅可满足上述要求,而且使萃取过程连续化。该装置主要由单口烧瓶、三颈烧瓶和热逆流提取器组成(图1)。     

改进的索氏萃取器在控制液固萃取终点时的应用

索氏萃取器是一种用有机溶剂从固体样品中连续萃取一定组分的仪器 ,在研究中药有效成分的提取方面有较为广泛的应用。但是用现有的索氏萃取器研究控制液固萃取终点时 ,只能在关闭热源待蒸馏瓶冷却下来后分析萃取室溶液中一定组分的含量 ,需要多次更换装有药粉的滤纸筒才能得到一组实验结果。这样既浪费时间 ,又消耗过多的费用。我们对索氏萃取器进行了改进 ,得到了一种便于控制液固萃取终点的索氏萃取器 (图 1 ) ,现以石油醚提取盾叶薯蓣水解残渣 (水解物 )中的薯蓣皂甙元为例介绍如下。图 1　改进的索氏萃取器　1　试剂与仪器　　 71 0型紫…     

咖啡因提取的综合性实验教学

介绍了一个综合性化学实验。该实验以绿茶为原料,95%的乙醇为提取剂,通过索氏提取器提取、常压蒸馏及升华等实验操作,得到咖啡因产品。通过超高效合相色谱法（Ultra Performance Convergence Chromatography,UPC2）确定咖啡因的含量,熔点测定法及1H-NMR归属分析表征结构。本实验将经典的有机化学实验和先进的分析测试仪器相结合,提高了学生的实验综合能力,激发了学生的科研兴趣和探索精神。     

一种简易植物提取装置的应用

介绍一种简易的植物提取装置及其在有机化学实验中的应用,并以茶叶中提取咖啡因为例具体说明该装置的操作方法及特点。     

油脂快速萃取装置萃取时间选择试验

3-86普及型油脂快速萃取装置是日本MRK公司的产品。该仪器对索氏提取器进行了改进,增加了煮沸萃取装置及程序定时器,使萃取时间大大减少,操作易于标准化。但对不同含油量的样品,说明书中没有     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Selective synthesis of 4,5-dihydroimidazo- and imidazo[1,5-a]quinoxalines via modified Pictet–Spengler reaction

An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction.     

Understanding the Diels-Alder reactivity of 1,2-azaborine analogues

The Diels-Alder reactivity of 1,2-heteroborines (H₄C₄B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed.