基础化学教学实验室试剂和仪器的科学细化管理

介绍了厦门大学化学国家级实验教学示范中心基础化学实验(一)实验室在试剂和仪器科学细化管理方面的一些具体做法,如试剂的排序存放、计划补充、优化使用及仪器的"五防"和"三位一体"管理模式。通过对试剂、仪器一系列规范、有序、科学的细化管理,节约了试剂用量,减少了废物排放量,保证了干净整洁的实验环境;培养了学生良好的实验习惯,保证了仪器的正常运行及获得准确的实验数据,并提高了仪器的使用寿命,为实验教学的顺利开展提供了有力的保障。希望能为国内高校化学教学实验室相关方面管理提供可借鉴的经验。     

以联席会和竞赛为载体构建实验教学改革交流的新平台——浙江省高校化学化工实验教学中心主任联席会暨化学学科(实验)竞赛10周年回顾

介绍成立浙江省高校化学化工实验教学中心联席会(以下简称:联席会)、举办化学学科(实验)竞赛的背景及发展情况。以联席会和竞赛为载体,建立了全省实验教学研究与改革的交流平台,扩大了实验教学示范中心的影响力和辐射面,推动了实验室建设、课程建设以及人才培养等各项工作,取得了丰硕的教学成果。     

“6S”在高校基础化学教学实验室细化管理中的灵活应用

主要介绍"6S管理"在厦门大学基础化学教学实验室内部细化管理过程中的应用实践与效果,特别是实验环境、物品定位管理、试剂管理、仪器管理等方面的具体做法,为高校化学教学实验室的建设和有效管理提供适应面广、操作性强的可借鉴经验。     

加强精细化管理 促进实验教学质量提高

实验室的日常管理水平直接反映了高校实验室管理的水平,也潜移默化地影响着实验教学的质量。为做好化学国家级实验教学示范中心的可持续性发展,详细介绍了吉林大学化学国家级实验教学示范中心在人员、设备、材料、环境和操作规程等精细化管理过程中所做的有别于其他学校的工作以及取得的良好效果,为实验室管理细节创新和促进实验教学质量提高积累了宝贵的经验。     

利用微信公众平台加强基础化学实验室管理的探索和实践

新媒体微信公众号具有简单、便捷、精准、可持续、学生乐于接受等特点,已渗透到高校学习、生活的每一个角落,也直接影响着高校实验室的信息化建设与管理。为了提高教学实验室的科学化管理水平,本文提出了利用微信公众号构建基础化学实验室管理系统,介绍了相关的应用与实践,这将使实验室管理和实验教学突破时空的限制,提高实验室利用效率,为实验教学和人才培养提供更高水平的服务。     

加强中学化学实验室管理的几点建议

化学实验室是进行化学实验教学,培养学生技能、开发智力的重要场所。实验室工作是学校教学工作的重要组成部分,因此,加强化学实验室的建设和管理,充分发挥实验室在化学教学工作中的作用,是提高教学质量的物质保证。     

加州大学圣迭戈分校的化学实验室安全管理与启示*

结合我国大学化学实验室的安全管理现状,介绍了加州大学圣迭戈分校化学实验室的安全管理经验,包括实验室安全管理制度、实验室准入、安全意识养成、安全巡查、试剂存放、危险品操作、废弃物处理以及实验室布局等方面。为国内高校的化学实验室安全管理提供借鉴。     

谈谈化学实验室的改建和科学管理

化学实验室是实现实验教学,全面完成化学教学任务的必不可少的基地,如何创造一个良好的基地,一是新建实验教学楼,二是在原有实验室的基础上,进行改造和扩充。无疑前者的办法需要花钱多,时间较长,见效则较迟。后一种办法比较适合大部分学校的实际,我们学校就是按第二种办法来改造和扩充实验室的,本文专谈我校化学实验室的改造、扩充和科学管理。     

强化无机及分析化学实验室管理工作的实践

介绍了南京林业大学化学基础教学实验中心无机及分析化学实验室强化管理工作的若干经验。实践表明,实验室的管理逐步走向了规范化、科学化,有利于更好地服务于实验教学,顺利完成各项实验教学任务。     

浅谈高校化学实验室的科学管理

随着高等学校教学改革的不断深入,对实验室管理工作提出了越来越高的要求。摆在我们面前的首要任务是管好、用好实验室,充分发挥实验室的整体效益,达到提高实验教学质量的目的。一、加强高校实验室管理的重要性实验室是高校的重要组成部分。随着教学改革的不断深入,实验室工作受到越来越多的重视,实验室工作水平成为反映高等学校教学水平、科研水平、管理水平的重要标志。国家教委正在组织、实施的对全国各高校实验室的评估工作,其中一项重要的指标就是各高校实验室管理的科学化水平。化学是一门实验性非常强的学科,在化学教学过程中…     

清除树脂在组合化学中的应用

清除树脂是一种特殊的固相试剂。近五年，它们被广泛的用于平行液相法合成组合化学库，简化液相组合化学库的纯化操作。本文综述了清除树脂在纯化操作中的使用策略。根据清除纯化原理，介绍了共价键型和离子键型两类清除树脂。给出了清除树脂在组合化学中的具体应用实例。最后对清除树脂的发展作了展望。     

GLARE: a new approach for filtering large reagent lists in combinatorial library design using product properties

We present a novel computer algorithm, called GLARE (Global Library Assessment of REagents), that addresses the issue of optimal reagent selection in combinatorial library design. This program reduces or eliminates the time a medicinal chemist spends examining reagents which a priori cannot be part of a "good" library. Our approach takes the large reagent sets returned by standard chemical database queries and produces often considerably reduced reagent sets that are well-behaved with respect to a specific template. The pruning enforces "goodness" constraints such as the Lipinski rule of five on the product properties such that any reagent selection from the resulting sets produces only "good" products. The algorithm we implemented has three important features: (i) As opposed to genetic algorithms or other stochastic algorithms, GLARE uses a deterministic greedy procedure that smoothly filters out nonviable reagents. (ii) The pruning method can be biased to produce reagent sets with a balanced size, conserving proportionally more reagents in smaller sets. (iii) For very large combinatorial libraries, a partitioning scheme allows libraries as large as 10(12) to be evaluated in 0.25 s on an IBM AMD Opteron processor. This algorithm is validated on a diverse set of 12 libraries. The results that we obtained show an excellent compliance to the product property requirements and very fast timings.     

Construction and Analysis of N-phosphoryl Peptide Libraries

N-Phosphoryl peptide libraries were constructed by transformation from homo-oligopeptide libraries, which was synthesized by self-assembly of amino acids with the assistance of phosphorus oxychloride. Electrospray ionization mass spectrometry (ESI-MS) was used to monitor the reaction.     

Global transformation of OBOC combinatorial peptide libraries into OBOC polyamine and small molecule libraries

In "one-bead-one-compound" (OBOC) combinatorial chemistry, a compound-bead library with hundreds of thousands to millions of diversities can be rapidly generated such that each bead displays only one chemical entity. The highly efficient "libraries-from-libraries" approach involves the global transformation of a peptide library into many small molecule solution-phase mixture libraries, but this approach has never been successfully applied to OBOC libraries. Here we report a novel approach that allows us to combine these two enabling technologies to efficiently generate OBOC encoded small molecule bead libraries. By using a topologically segregated bilayer bead and a "ladder-synthesis" method, we can prepare peptide libraries with the peptide on the bead surface and a series of peptide ladders in the bead interior. Various global transformation reactions can then be employed to transform the starting peptide library into a variety of peptidomimetic libraries. During the transformation reactions, the peptide ladders in the bead interior are also transformed in a predictable manner. As a result, individual compound bead can be decoded by analyzing the hydrogen fluoride-released encoding tags with matrix-assisted laser desorption ionization Fourier transform mass spectrometry. Using this novel approach, a random encoded dipeptide library was prepared and subsequently transformed into polyamine and poly- N-acetylamine sublibraries. Random beads isolated from these sublibraries were reliably decoded.     

Highly enantioselective direct alkylation of arylacetic acids with chiral lithium amides as traceless auxiliaries

A direct, highly enantioselective alkylation of arylacetic acids via enediolates using a readily available chiral lithium amide as a stereodirecting reagent has been developed. This approach circumvents the traditional attachment and removal of chiral auxiliaries used currently for this type of transformation. The protocol is operationally simple, and the chiral reagent is readily recoverable.     

A Chemistry for Incorporation of Selenium into DNA-Encoded Libraries

Conventional direct C−H selenylation suffers from simple selenation with limited atom economy and complicated reaction system. In this work, we designed benzoselenazolone as a novel bifunctional selenide reagent for both off- and on-DNA C−H selenylation under rhodium(III) catalysis. We show that using benzoselenazolone allowed production of a series of selenylation products containing an adjacent aminoacyl group in a fast and efficient way, with high atom economy. The synthetic application of this method was demonstrated by taking advantage of the amide functionality as a nucleophile, directing group, and amide coupling partner. This work shows great potential in facilitating rapid construction of selenium-containing DNA-encoded chemical libraries (SeDELs), and lays the foundation for the development of selenium-containing drugs.     

Practical aspects of Fourier transform and correlation based processing of spectrochemical data

Fourier transform based signal processing methods are beginning to be widely used for the treatment of spectrochemical data. The most common approach to Fourier transformation is through the utilization of the so called Fast Fourier Transform algorithm or FFT as it is usually designated. However, several versions of the FFT abound in the literature and in program libraries and many subtleties exist with respect to data pre-treatment, data post-treatment, inverse Fourier transformation and manipulation of real and imaginary arrays that can cause considerable grief to the uninitiated. In this presentation numerous examples will be presented illustrating several practical aspects of implementing FFT's and cross-correlations (Fourier transform route) on spectrochemical data sets. Particular attention is paid to the manipulation to the input and output real and imaginary arrays.     

Convenient and efficient method for the synthesis of substituted quinolines via one-pot heteroannulation reaction of o-amino arylketones with α-methylene ketones under solvent-free conditions

A facile and practical approach to the synthesis of a wide range of functionalized quinolines was developed via a tandem heteroannulation reaction of o-aminoarylketones with diverse α-methylene ketones in high yields by using tetrabutylammonium peroxydisulfate as a versatile reagent (25?mol%) at ambient temperature under solvent-free conditions. This protocol was applied to the synthesis of drug-like molecules, which are key intermediates of alkaloid camptothecin.     

A Chemistry for Incorporation of Selenium into DNA‐Encoded Libraries

Conventional direct C?H selenylation suffers from simple selenation with limited atom economy and complicated reaction system. In this work, we designed benzoselenazolone as a novel bifunctional selenide reagent for both off‐ and on‐DNA C?H selenylation under rhodium(III) catalysis. We show that using benzoselenazolone allowed production of a series of selenylation products containing an adjacent aminoacyl group in a fast and efficient way, with high atom economy. The synthetic application of this method was demonstrated by taking advantage of the amide functionality as a nucleophile, directing group, and amide coupling partner. This work shows great potential in facilitating rapid construction of selenium‐containing DNA‐encoded chemical libraries (SeDELs), and lays the foundation for the development of selenium‐containing drugs.     

Ru(II)-Catalyzed Hydroarylation of in situ Generated 3,3,3-Trifluoro-1-propyne by C−H Bond Activation: A Facile and Practical Access to β-Trifluoromethylstyrenes

In this study, a practical and straightforward synthesis of β-(E)-trifluoromethylstyrenes by ruthenium-catalyzed C−H bond activation was developed. The readily available and inexpensive 2-bromo-3,3,3-trifluoropropene (BTP), a non-ozone depleting reagent, was used as a reservoir of 3,3,3-trifluoropropyne. With this approach, the monofunctionalization of a panel of heteroarenes was possible in a safe and scalable manner (23 examples, up to 87 % yield). Mechanistic investigations and density functional theory (DFT) calculations were also conducted to get a better understanding of the mechanism of this transformation. These studies suggested that 1) a cyclometallated ruthenium complex enabled the transformation, 2) this complex exhibited high efficiency in this transformation compared to the commercially available [RuCl₂(p-cymene)]₂ and 3) the mechanism proceeded through a bis-cyclometallated ruthenium intermediate for the carboruthenation step.