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...     

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…     

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)。     

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     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

Copper catalyzed/mediated synthetic methodology for ebselen and related isoselenazolones

Scope of the copper catalyzed/mediated selenium-nitrogen coupling reaction has been studied for the synthesis of isoselenazolones. It is noticed that the 2-chloro, 2-bromo-, and 2-iodo-aryl amides substrates can be exploited in the selenium-nitrogen coupling reaction by employing 25-100 mol % of CuI/1,10-phenanthroline (L) and potassium carbonate as a base in DMF. Furthermore, electron rich 2-chloro-arylamides also underwent selenium-nitrogen coupling reaction to give biologically important selenium-nitrogen heterocycles. Also, copper-catalyzed selenium-nitrogen coupling reaction has been meticulously applied for the synthesis of diaryl diselenides having methoxy, amine, and amide functionality from respective aryl iodides in the presence of stoichiometric amount of succinimide as an external Se-N coupling partner.     

Knoevenagel condensation catalyzed by novel Nmm-based ionic liquids in water

A series of novel N-methyl morpholine (Nmm) based ionic liquids with 1,2-propanediol group were synthesized and used as catalysts for Knoevenagel condensation at room temperature in water. Under the effect of the catalyst, various aldehydes or aliphatic ketones could react with a wide range of activated methylene compounds well, including malononitrile, alkyl cyanoacetate, cyanoacetamide, β-diketone, barbituric acid, 2-arylacetonitrile and thiazolidinedione. Furthermore, most of the products could be separated just by filtrating and washing with water. Additionally, the catalyst is recyclable and applicable for the large-scale synthesis.     

Construction of polyheterocyclic spirotetrahydrothiophene derivatives via sulfa-Michael/aldol cascade reaction

A series of polyheterocyclic spirotetrahydrothiophene derivatives were obtained in moderate to excellent yields via a catalyst-free sulfa-Michael/aldol cascade reaction of chalcones 1 and commercially available 1,4-dithiane-2,5-diol 2 under mild conditions. We also present the first asymmetric sulfa-Michael/aldol cascade reaction of chalcones 1 and commercially available 1,4-dithiane-2,5-diol 2 with moderate to good enantioselectivities catalyzed by readily available chiral phase-transfer catalysts (PTCs).     

Suzuki-Miyaura reactions of the soluble guanylate cyclase inhibitor NS2028: a non-product specific route to C-8 substituted analogues

Both soluble guanylate cyclase (sGC) inhibitors ODQ 1 and NS2028 2 are synthesized via improved protocols. In the former case treating 3,4-dihydroquinoxalin-2(1H)-one oxime 8, which can be prepared in two steps from 1,2-benzenediamine, with 1,1′-carbonyldiimidazole (CDI) gives the dihydro-ODQ 10 that in the presence of KMnO₄ oxidises to give ODQ 1 in an overall yield of 46% starting from 1,2-benzenediamine. In the latter case, the synthesis affords NS2028 2 from 2-amino-4-bromophenol 3 in three steps with an overall yield of 85% and avoids the need for chromatography. Furthermore, Suzuki-Miyaura reaction conditions are described that enable the preparation of 8-aryl and 8-heteroaryl derivatives of NS2028 directly from NS2028 2. Finally, demethylation of the 8-(methoxyphenyl) substituted analogues afforded the 8-(hydroxyphenyl) derivatives 40-42. All new products are fully characterised.