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8-氨基喹啉及其衍生物是近年来正在开发的一类新试剂。笔者合成的5-〔(4-乙酰氨基苯基)偶氮〕-8-氨基喹啉(AAPAQ),又是8-氨基喹啉的一个新的衍生物。AAPAQ用于钯的测定,灵敏度较高,选择性较好,用于水相光度法直接测定试样中的微量钯,结果满意。合成方法:①重氮化反应,将1.5g对乙酰氨基苯胺,5ml浓盐酸及10ml水混合,用冰浴冷至0℃,在不断搅拌下,滴加含0.79mol·L~(-1)亚硝酸钠的8ml水溶液。在0.5℃持续搅拌30min,使重氮化完全。②偶联反应,将①的重氮盐溶液滴至含有1.4g 8-氨基喹啉的60ml HAc-NaAc缓冲溶液中,补加NaOH溶液,保持pH5～6之间,低温偶合1.5h,抽滤,得粗品,用吡啶-乙醇-水(1:5:1)混合溶剂重结晶,得橙色针状晶体.晶体经元素分析,红外光谱测定,鉴定为5-〔(4-乙酰氨基苯基)偶氮〕-8-氨基喹啉。
8-Aminoquinoline and its derivatives are a new class of reagents under development in recent years. The synthetic 5 - [(4-acetamidophenyl) azo] -8-aminoquinoline (AAPAQ) is a new derivative of 8-aminoquinoline. AAPAQ for the determination of palladium, high sensitivity, better selectivity for the determination of trace palladium in aqueous phase spectrophotometry, with satisfactory results. Synthesis method: ① diazotization reaction, 1.5g of acetamidoaniline, 5ml concentrated hydrochloric acid and 10ml of water were mixed, cooled to 0 ° C with an ice bath, with constant stirring, dropwise with 0.79mol · L ~ (-1) Sodium nitrite in 8 ml of water. Stirring was continued at 0.5 ° C for 30 min to complete diazotization. ② coupling reaction, the diazonium salt solution ① drops containing 1.4g 8-aminoquinoline 60ml HAc-NaAc buffer solution, add NaOH solution, maintaining pH5 ~ 6, low temperature coupling 1.5h, suction filtration The crude product was recrystallized from a mixed solvent of pyridine - ethanol - water (1: 5: 1) to obtain orange needle crystal.The crystal was identified as 5 - [(4 - acetamidophenyl) Azo] -8-aminoquinoline.