化学合成。
有机合成; 医药中间体
合成路线 1(1. 合成:2536-35-8)
产率:88%
合成条件:With sodium hydroxide; sulfuric acid; nitrogen; hydrogen bromide In acetic acid
实验步骤:16-溴十六烷酸2的合成向装有机械搅拌器,回流冷凝器和氮气入口的2升三颈圆底烧瓶中加入177g(0.63摩尔)16-羟基十六烷酸1.向该容器中加入1000mL(5摩尔)30%溴化氢的乙酸溶液和310mL浓硫酸。该系统配备有顺序捕集器,其包含氢氧化钠颗粒捕集器,25%氢氧化钠水溶液捕集器和饱和碳酸钠捕集器。将反应物在室温下搅拌过夜,然后将其加热回流6小时。冷却反应混合物,倒入冰水中,真空过滤沉淀的固体。在高真空下干燥后,得到196g的16-溴十六烷酸。产率:88%纯度:> 95%熔点:67°-69℃.DSC = 69.0℃(急)IR(nujol mull):1700(s),650(s)1 H NMR(200MHz,CD2 CL2) ):δ3.4(t,J = 8 Hz,2H),2.3(t,J = 8 Hz,2H),1.8(m,2H),1.6(m,2H),1.2(br.s,22H)
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