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8-羟基喹啉-5-甲醛和8-羟基喹啉-5-磺酸联产工艺研究

Study on the Process of Joint Production of 8-Hydroxyquinoline-5-Carbaldehyde and 8-Hydroxyquinoline-5-Sulphonic Acid
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摘要 以8-羟基喹啉为原料,在酸性条件下与水合氯醛发生缩合反应得到5-(α-羟基-β-三氯)-8-羟基喹啉(I),联产8-羟基喹啉-5-磺酸(II)。(I)在碱性条件下水解生成8-羟基喹啉-5-甲醛(III),产物经熔点仪、元素分析仪、液-质联用仪、红外光谱仪及核磁共振氢谱等进行表征。探讨了反应温度、反应时间、原料比、溶剂及溶剂的重复性等因素对实验的影响。确定产物(I)的最佳反应条件为:n(8-羟基喹啉)∶n(水合氯醛)∶n(硫酸)=1∶1.2∶4.6,反应温度为80℃,反应时间为12 h,产物收率为55%;产物(III)的最佳反应条件为:n(I)∶n(KOH)=1∶5.1,回流反应7 h,收率为21%。 5 - ( α - hydroxy - β - trichloroethyl) - 8 - hydroxyquinoline ( Ⅰ), 8 - hydroxy quinoline - 5 - sulfohie acid (Ⅱ) was synthesized by reaction of 8 -hydroxyquinoline with chloral hydrate when sulfuric acid was used as solvent. 8 -hydroxylquinoline -5 -carbaldehyde was synthesized by reaction of (Ⅰ) with KOH in methanol. The structure of resultant was characterized with melting point detector, elemental analyzer, LC - MS, IR and 1 H NMR. The effects of temperature, reaction time, volumes of solvents, material ratio and reusability of solvents on the reaction were studied. The optimum conditions of (Ⅰ) were found as follows : n (8 - hydroxyquinoline) : n ( chloral hydrate) : n (H2SO4) = 1: 1.2: 4.6, reaction temperature 80℃, reaction time 12 h, the yield of (Ⅰ) was 55 %. The optimumconditions of(Ⅲ) were found as follows : n(Ⅰ) : n(KOH) = 1: 5.1, reaction time 7h under reflow, the yield of (Ⅲ) was 21%.
出处 《化工时刊》 CAS 2013年第10期1-5,共5页 Chemical Industry Times
基金 国家海洋公益性行业科研(201305007) 江苏省高校产业化推进项目(JHB2011-60) 江苏省六大人才高峰资助项目(2009年) 江苏省高校优势学科建设工程资助项目 连云港市产学研联合研究项目(CXY1212)
关键词 8-羟基喹啉-5-醛 8-羟基喹啉-5-磺酸 8-羟基喹啉 水合氯醛 联产 8 - hydroxyquinoline - 5 - carbaldehyde 8 - hydroxyquinoline - 5 - sulphonic acid 8 -hydroxyquinoline Chloral hydrate joint production
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