摘要
以α-萘胺为起始原料，通过封管反应、碱提取、水蒸气蒸馏、乙酸酸化和乙醇重结晶，取得了纯度较高的2-巯基-β-萘并噻唑。研究发现，2-巯基-β-萘并噻唑与PdCl2有高灵敏度、高选择性的络合显色作用，并把这种显色方法成功地用于该噻唑的提纯检验上。对2-乙硫基-β-萘并噻唑的物态提出了不同看法，得到IR谱的证明。最终在2-乙硫基-β-萘并噻唑与硫酸二乙酯摩尔比1：1．5～1：1．8，反应温度110～130℃的优化反应条件下成功合成了2-乙硫基-β-萘并噻唑乙替硫酸-酯盐，产率34％，m．P．52～54℃。
The high purity of 2-mereapto-β-naphthothiazole was obtained with α-naphthylamine as raw material via reaction of seal glass tube, alkaline extraction, vapor distillation, acidification of acetic acid and ethanol recrystallization. The research displays a chromogenic complex action of high sensitivity and better selectivity with PdCl2, the chromogenic method was applied to the purification and test of naphthothiazole successfully. A different view for the physical state of 2-ethylmereapto-β-naphthothiazole was presented, which was proved by IR spectrum. 2-Ethylmercapto-β-naphthothiazole etho-ethylsulfate was successfully synthesized under the conditions of molar ratio of 2-ethylmereapto-β-naphothiazole to ethyl sulfate 1 ： 1.5 ～ 1 ： 1.8 and reaction temperature 110 ～ 130 ℃ . The yield of product is 34% ,m. p. 52 ～54 ℃.
出处
《应用化工》
CAS
CSCD
2008年第8期861-864,共4页
Applied Chemical Industry
基金
陕西省自然科学基金项目(96H07)
