【摘要】 以1-氨基-2-苯氧基-4-羟基蒽醌、氯磺酸、氯化亚砜、3-乙氧基丙胺为原料及Na2CO3为缚酸剂合成了C.I.分散红92。研究了氯磺酸、氯化亚砜用量及温度对氯磺化的影响,研究了3-乙氧基丙胺用量、pH值及温度对胺化缩合的影响。通过实验得到了较佳的反应条件,原料摩尔比是1-氨基-2-苯氧基-4-羟基蒽醌:氯磺酸:氯化亚砜:3-乙氧基丙胺为1:8:0.6:1;氯磺化温度为30℃～35℃;胺化缩合pH值为7～8,温度为15℃～20℃。并通过HPLC、1H-NMR、IR和MS对目标产品进行了分析。以1-氨基-2-苯氧基-4-羟基蒽醌计,总收率大于91%,目标产品HPLC纯度大于99%,溶剂回收率为95%。更多还原

【Abstract】 Using 1-amino-2-phenoxy-4-hydroxyanthraquinone,chlorosulfonic acid,thionyl chloride,and 3-ethoxypropylamine as raw materials and sodium carbonate as acid-binding agent,C.I.Disperse Red 92 was synthesized.The efects of amount of chlorosulfonic acid,thionyl chloride,and reaction temperature on the yield of C.I.Disperse Red 92 in the sulfonate and chlorination were investigated.The effects of amount of 3-ethoxypropylamine,pH,and reaction temperature on the yield of C.I.Disperse Red 92 in the amidation and hydrysis were studied.The better reaction condition was obtained by experiments,the raw materials molar ratio of 1-amino-2-phenoxy-4-hydroxyanthraquinone:chlorosulfonic acid:thionyl chloride:3-ethoxypropylamine was found to be 1:8:0.5:1;the sulfonate and chlorination process reaction temperature was 30～35℃;the amidation process reaction pH was 7～8,reaction temperature was15～20℃.The destination product was identified by HPLC,1H-NMR,IR and MS.Its total yield was over 91% by1-amino-2-phenoxy-4-hydroxyanthraquinone and over 99% purity was obtained.The recovery of solvent was 95%.更多还原