A new method for synthesizing eltoprazine is presented in this article.3-nitrobenzene-1,2-diol is synthesized with pyrocatechol via a nitrating reaction,and then we use 1,2-dibromoethane as the cycling agent to prepare 5-nitro-2,3-dihydrobenzo[b]dioxine.5-amino-2,3-dihydrobenzo[b]dioxine is synthesized with 5-nitro-2,3-dihydrobenzo[b]dioxine via a reductive reaction in ethanol using hydrazine hydrate as reductive agent and Pd/C as catalyst.The object product eltoprazine is then prepared by a cycling reaction using bis(2-chloroethyl)ammonium chloride.This method could be easy to operate in laboratory and get a high yield.
该文制备了一种新型吸附材料三乙烯四胺修饰β-环糊精交联树脂（TETA-β-CDP）,并对其进行红外光谱表征,优化了该吸附材料对痕量铅、镉的吸附和解析条件,建立了动态条件下同时分离富集/原子吸收光谱测定大米中铅和镉的新方法。在p H 5.5时,样品溶液以1.0 m L/min流速过柱,试液中的Pb2＋和Cd2＋可被该树脂定量富集,其动态饱和吸附容量分别为22.8,31.3 mg/g,吸附在TETA-β-CDP上的Pb2＋和Cd2＋可用0.1 mol/L HCl以0.8 m L/min流速完全洗脱。该方法对铅、镉的检出限（3σ,n=11）分别为0.038 mg/L和0.016 mg/L;线性范围分别为0.2~20 mg/L和0.05~2.5 mg/L;相对标准偏差（RSD）分别为2.8%和1.7%;加标回收率分别为97.5%~101.0%和95.0%~102.5%。该方法用于大米样品中痕量铅、镉的测定,结果满意。
