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N-苯基-4-羟基苯甲酰胺的制备

时间:2021-01-16 13:19来源:毕业论文
以对羟基苯甲酸和氯化亚砜为原料,N,N-二甲基甲酰胺(DMF)和苯为溶剂,制备了中间体对羟基苯甲酰氯。考察了溶剂配比、氯化时反应温度、反应时间、氯化亚砜和对羟基苯甲酸的摩尔

摘要:以对羟基苯甲酸和氯化亚砜为原料,N,N-二甲基甲酰胺(DMF)和苯为溶剂,制备了中间体对羟基苯甲酰氯。考察了溶剂配比、氯化时反应温度、反应时间、氯化亚砜和对羟基苯甲酸的摩尔投料比对收率的影响,确定了较佳的工艺条件为:反应温度为60℃,反应时间为5h,n(对羟基苯甲酸):n(氯化亚砜)=0.072:0.168,n(苯):n(氯化亚砜)=0.789:0.168,在此条件下,对羟基苯甲酰氯的产率达90%。再由中间体对羟基苯甲酰氯和苯胺反应,以DMF为溶剂,制备了目标产物N-苯基-4-羟基苯甲酰胺。考察了溶剂配比、反应时间、反应温度、摩尔投料比对目标产物收率的影响,确定了较佳的工艺条件为:反应温度为60℃,反应时间4h,n(苯胺):n(对羟基苯甲酰氯)=0.423:0.168,在此条件下,目标产物的产率达55%,其熔点200.0~200.4℃。经红外光谱分析(IR)及核磁共振(1HNMR)进行了表征,产物为N-苯基-4-羟基苯甲酰胺。62213

毕业论文关键词: 氯化亚砜;对羟基苯甲酰氯;N-苯基-4-羟基苯甲酰胺

Preparation of N- pheNyl-4-hydroxypheNyl-carboxamide

Abstract:Hydroxybenzoic acid and thionyl chloride as raw material, N, N- dimethylformamide (DMF) and benzene as solvent for the preparation of the intermediate-hydroxybenzoyl chloride. The effects of solvent ratio, reaction temperature, reaction time, thionyl chloride and parabens molar feed ratio on when chlorination yield determined optimum conditions: the reaction temperature is 60℃, reaction time was 5h, n (p-hydroxybenzoic acid): n (thionyl chloride) = 0.072: 0.168, n (benzene): n (thionyl chloride) = 0.789: 0.168 under these conditions, paraben chloride yield of 90%Then the intermediate of the reaction of aniline and hydroxybenzoyl chloride, DMF as the solvent, the desired product was prepared N- phenyl-4-hydroxybenzamide. The effects of solvent ratio, reaction time, reaction temperature, the molar feed ratio on the yield of the target, determine the optimum conditions are as follows: for reaction temperature is 60℃, reaction time 4h, n (aniline) hydroxybenzoyl chloride) = 0.423: 0.168 under these conditions, the yield was 55%of the desired product, mp 200.0 ~ 200.4 ℃. By infrared spectroscopy (IR) and nuclear magnetic resonance (1HNMR) were used to characterize the product was N- phenyl-4-hydroxy-carboxamide.

Keywords: Thionyl chloride; chloride paraben; N- phenyl-4-hydroxybenzamide

目  录

1.引言 1

1.1 世界农药发展趋势 1

1.2 农药有机合成进展 1

1.3 文献综述 4

1.3.1 酰胺类化合物 4

1.3.2 苯甲酰氯的应用前景 5

1.3.3 苯甲酰氯的合成 5

1.4 本文研究内容 6

2.实验部分 8

2.1 实验仪器与试剂 8

2.1.1 实验仪器 8

2.1.2 实验的试剂及其物性常数 9

2.2实验步骤 9

2.2.1 对羟基苯甲酰氯的制备 9

2.2.2 N-苯基-4-羟基苯甲酰胺的制备 9

2.2.3 N-苯基-4-羟基苯甲酰胺的提纯(重结晶) 10

3.结果与讨论 11

3.1 对羟基苯甲酰氯的制备 11

3.1.1 反应温度对对羟基苯甲酰氯收率的影响 N-苯基-4-羟基苯甲酰胺的制备:http://www.751com.cn/huaxue/lunwen_68347.html

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