【作者】 李倩；

【导师】 戴立言；

【作者基本信息】 浙江大学 ， 化学工程， 2010， 硕士

【摘要】 Octopirox是一种新型去屑止痒剂,其去屑止痒性能优于同类去屑止痒剂。它不仅能够与洗发水的其他添加成分较好的混合,而且无毒无刺激,安全性能较高,因此是一种具有极大推广价值的去屑止痒剂。本文在研究文献合成方法的基础上,对合成Octopirox的关键中间体的合成进行了研究。本文参考类似结构化合物的合成方法,确定了一条收率较高且操作方便的路线,以3,5,5-三甲基已酰氯和3-甲基-2-丁烯酸甲酯为起始原料,经酰氯化、F-C酰基化、水解和内酯化反应制备4-甲基-6-(2,4,4-三甲基戊基)-2-吡喃酮,总收率52%。实验中考察了各步反应中催化剂用量、反应温度、投料比等对反应的影响,确定了最佳工艺条件。另外,本文对合成Octopirox相关化合物的比热容进行了测定,实验采用冷却法,利用改造的简易量热器,在常压下和308.15～333.15K的温度范围内测定了乌洛托品-醋酸、醋酸酐-醋酸体系不同组成下的比热容,测得的C_p值与温度和浓度进行关联,其实验值与计算值的RMSD分别为1.47%和0.46%。对于醋酸酐-醋酸体系,由C_p值计算出摩尔超额比热容,将C_p~E值用Redlich-Kister方程进行关联,由此得出的计算值与实验值的AAD为5.68%。更多还原

【Abstract】 Octopirox is a kind of powerful anti-dandruff agent with advantages on removing dandruff over other ones.It has good cooperation with other components of shampoo.And it is safe to people with no stimulation,no toxic.So,Octopirox has great application value.In this study,a synthesis route with higher yield and practicable operation has been chosen based on synthesis method of similar compounds for 4-methyl-6-(2,4,4-trimethylpentyl)-2-pyrone,which is an important intermediate of Octopirox.It is prepared with 3,5,5-trimethyl hexanoyl chloride and methyl 3-methyl-2-butenoate by acyl chlorination,F-C acylation, hydrolysis and lactonization,reaction,and the total yield is 52%.The effects of temperature, amount of catalysts and the ratio of substrate in each step have been investigated,and the suitable conditions for the process have been obtained.And also,heat capactites for correlated compounds of synthesis of Octopirox have been studies in this paper.Heat capacities of binary mixtures of acetic acid with acetic anhydride and methenamine were measured by cooling method with a simple calorimeter from 308.15 K to 333.15 K at atmospheric pressure with different compositions.The values of C_p is correlated with temperatures and molar fraction,and the RMSD between the experimental and calculated values is 0.46%and 1.47%separately.The excess molar heat capacities C_p~E of the binary mixture of acetic acid with acetic anhydride were calculated from the experimental data,and were fitted to the Redlich-Kister equation,and the AAD between experimental and calculated values is 5.68%.更多还原