微波组合化学在新药研究中的应用

微波组合化学是组合化学快速发展的结果。与传统方法下的组合化学相比 ,微波组合化学加快了新药筛选中化合物库的建立过程 ,是 1种切实有效的有机合成新技术 ,并且形成了多种合成方法。本文对近 10年来出现的微波组合化学方法及其在新药研究中的应用进行了简单的综述。

Design and Synthesis of Novel Fluorine-containing Acrylates

A series of novel fluorine-containing acrylates 6a-6g were synthesized via the condensation of ethyl cyanoacetate and trifluoroacetic anhydride, followed by chloridization and the coupling reaction with amines. These new compounds exhibited some biological activity as preliminary bioassay indicated. A plausible reaction mechanism was outlined and discussed.

Synthesis of lithium difluoro(oxalate)borate(LiODFB), phase diagram and ions coordination of LiODFB in dimethyl carbonate

A new two-step synthetic method was successfully developed to simplify the recrystallization process of lithium difluoro(oxalate)borate(LiODFB).Meanwhile,the purity of LiODFB as-prepared was determined by NMR,ICP-AES and Karl Fisher measurements,respectively.The as-prepared LiODFB presents a high purity up to 99.95%.Its metal ions and water contents are under good control as well.Besides,its structure information and thermal properties were confirmed by FTIR,Raman and DSC-TGA analyses,respectively.LiODFB exerts fine thermostability and hypo-water-sensitivity and its structure information agrees well with previous literature.Furthermore,a combination of phase diagram and Raman spectroscopy were utilized to study the thermal phase behavior and ions coordination of LiODFB-DMC binary system to optimize the synthesis and recrystallization process.Although there are three types of molecular interaction forms(CIPs,AGG-IIa,AGG-IIIb)in LiODFB-DMC binary system,LiODFB can only be isolated as large single crystal solvate as LiODFB·(DMC)3/2 by slowly cooling subjected to the nucleation kinetics.Therefore,the fundamental information of our work is helpful in accelerating the application of LiODFB in Li-ion secondary batteries.

A novel synthesis of fluvoxamine maleate

Fluvoxamine maleate is an excellent antidepressive drug. In the literatures, it was synthesized by the use of 4-（trifluoromethyl） aniline or 4-（trifluoromethyl） benzonitrile as starting materials and 5-methoxy-4＇-（trifluoromethyl-phenyl） valerophenone as a key intermediate. However, the methods in literatures have some disadvantages, such as the use of expensive materials, heavy pollution of environment, long reaction time and low yield of the product （only 30-40% overall yield）. We herein report an environmentally friendly synthetic method of fluvoxamine maleate, which used 4-（trifluoromethyl） benzoic acid and tetrahydrofuran as starting materials and FeCI3 as catalyst for the coupling of acid chloride with Grignard reagent. The fluvoxamine maleate was synthesized in 46% overall yield, through the oximation, etheration and salification of the intermediate successively.This method has some advantages, such as the use of commercially available materials, low cost, short production period （12-14 h）, high yield and light pollution.

500微米沸石分子筛单晶的制备方法

介绍了 2 0世纪 90年代以来 5 0 0 μm以上的沸石分子筛单晶的六种制备方法 ,包括类区域融化法、植入晶种法、有机热合成法、块状原料溶解法、氟离子效应合成法和双硅源法。这些方法通过控制反应体系中晶核的形成数量 。