对羟基苯甲酰氯的制备+文献综述
关键词：对羟基苯甲酰氯；对羟基苯甲酸；酰氯化
The preparation of p-hydroxy benzoyl chloride
Abstract: Taking p-hydroxy benzoic acid(solid) as raw material,using benzene as solvent,N, N-dimethyl formamide (DMF) as cosolvent, stir to dissolve,heating up to 30℃ while stirring.Within 0.5h,slowly and dropwise adding thionyl chloride and. Add over,around 45℃ heat preservation reaction in 4h,preparation of p-hydroxy benzoyl chloride.Then cool,the reaction was allowed to stand for separation,the upper of N,N-dimethyl formamide and its hydrochloride,and a small amount of impurity of hydroxyl benzoyl chloride,the lower of benzene solution of p-hydroxy benzoyl chloride and a small amount of N,N-dimethyl formamide(DMF).Take the lower liquid,45℃ steam recycling thionyl chloride,N,N-dimethyl formamide(DMF) and parts of benzene,cooling of hydroxy benzoyl chloride precipitation purpose products.Focuses on the drop of the acyl chlorination agent addition amount, temperature and drops plus time,reaction temperature,time and feeding molar ratio influencing on the yield of p-hydroxy benzoyl chloride, objective product, rom the choice of the preparation conditions of hydroxy benzoyl chloride respectively: drop temperature ( T1= 30 ℃ ),and drop time( t1= 0.5 h ),and reaction temperature( T2= 45 ℃ ),and reaction time( t2 = 4 h ),M( p-hydroxy benzoic acid ):M( benzene ):M( DMF ):M( sulfide sulfoxide ) =1:5.4:1.85:2.
KeyWords: p-hydroxy benzoyl chloride;p-hydroxy benzoic acid;acylation
目录
1 绪论 1
1.1 课题依据 1
1.2 课题介绍 1
1.2.1 课题的背景 1
1.2.2 酰氯的主要应用研究及进展 2
1.2.3 酰胺类除草剂 3
1.2.4 酰胺作为农药的发展 5
1.3 农药业国/内外的发展和研究 6
1.3.1 农药在国内发展的现状 6
1.3.2 农药在国外发展的现状 6
1.4 酰氯在医药中的应用 7
1.4.1 医药的国际市场 7
1.4.2 医药的国内市场 8
1.5 酰氯的合成方法 8
1.5.1 氯化亚砜法 8
1.5.2 氯化磷法 9
1.5.3 其他氧化方法 10
1.6 其他酰氯类化合物 10
1.6.1 苯甲酰氯 10
1.6.2 对氟苯甲酰氯 11
1.6.3 对氯苯甲酰氯 11
1.6.4 邻、间、对苯二甲酰氯 12
2 实验部分 13
2.1 实验仪器与试剂 13
2.1.1 实验仪器 13
2.1.2 试剂及其物性常数 14
2.2 实验内容 14
2.2.1 对羟基苯甲酰胺的制备 14
3 结果分析与讨论 15
3.1 溶剂的量对产率的影响 15