对氨基苯偶氮巴比妥酸制备及偶合反应研究
关键词：颜料；乙酰乙酰苯胺；对硝基苯胺；巴比妥酸；对氨基苯偶氮巴比妥酸
The Preparation And The Research Of Coupling Reaction Of 4-aminobenzoic-azo-Barbituricacid
Abstract：The Barbituricacid provided by the corporation is used to be coupled with p-nitroaniline, through which mono azocompounds—p-nitrobene azo barbituricacid (A) can be generate. After that, (A) and sodium sulfide have reduction and finally produce the compound of 4-aminobenzoic-azo-Barbituricacid(B). Since the structure of（B）contains multiple amido groups and azo groups, it can be coupled with Acetoacetanilide which is the coupling component of the industrial pigment, and produce the 4-[[(4- acetoacetanilideazo)PHenyl]azo]- Barbituricacid (C) which is the compound containing disazo groups and multiple amido groups. Compared with ordinary pigment, (C) has great improvements in terms of light resistance, solvent resistance, stability and tinting strength. The result of experiment illustrate the best reaction condition of (A): the diazotization reaction: PH＜1, nHCl :nNaNO2:nB=3.5:1.2:1.0, 10℃,40min; the coupling reaction: PH=9, nHCl:nNaNO2 :nB:nA =3.5:1.2:1.0:1.2, 10℃,50min. The best reaction condition of (B) is PH= 8, nC :nNa2S = 1.0:1.7, 75℃, 10h. The best reaction condition of (C) is: the diazotization reaction: 在PH＜1, nH2SO4:nNaNO2:nB=152.1:1.4:1.0, 5℃, 50min; the coupling reaction: PH=5.5~6, nEDTA:nNaOH:nB:nA =0.4:2.14:1.0:1.3, 8℃, 60min. Use 1HNMR, IR spectroscopy, etc. to characterize the structure of (B) and (C).
KeyWords：pigment；bisdiazo；Acetoacetanilide；4-Nitroaniline；Barbituricacid
目 录
1引 言 1
1.1 研究依据 1
1.2 原料及中间体的结构及性质 1
1.2.1 巴比妥酸的结构及性质 1
1.2.2 N-乙酰乙酰苯胺的结构及性质 2
1.2.3 对氨基苯偶氮巴比妥酸的结构及性质 3
1.3 文献综述 4
1.3.1双偶氮颜料的合成方法[1] 4
1.3.2 重氮化反应 5
1.3.3 偶合反应[9] 7
1.3.4 氨基苯偶氮巴比妥酸合成路线 11
1.3.5 4-乙酰乙酰苯胺偶氮基苯偶氮巴比妥酸 12
1.4 研究内容 13
2 实验 14
2.1对氨基苯偶氮巴比妥酸的合成制 14
2.1.1 药品及仪器 14
2.1.2 对氨基苯偶氮巴比妥酸的合成 15
（1）氯化硝基重氮苯的合成 15
2.1.3 对氨基苯偶氮巴比妥酸的结构表征 15
2.2 4-乙酰乙酰苯胺偶氮基苯偶氮巴比妥酸的合成研究 18
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