化学合成。
化学合成
合成路线 1(1. 合成:1123-93-9)
产率:52%
合成条件:Stage #1: With tin(ll) chloride In isopropyl alcohol for 24 h; Heating / reflux Stage #2: With sodium hydroxide In water; isopropyl alcohol
实验步骤:将5-NITRO-1,3-苯并噻唑(描述5,1.9g,11mmol)和氯化锡(II)二水合物(8.6g,38mmol)在2-丙醇(30ml)中的混合物加热至回流 持续24小时。 将冷却的反应混合物倒入冰/水混合物(85ml)中并用氢氧化钠调节至pH7。 用乙酸乙酯(3×50ml)萃取混合物,合并的有机层用硫酸钠干燥,过滤并蒸发。 残留物通过硅胶柱色谱纯化(洗脱剂1:1己烷:乙酸乙酯),得到1,3-苯并噻唑-5-胺(820mg,52%)。 LHNMR(CDCL3)6 6.85(1H,dd,J2.3,8.6),7.40(1H,d,J2.1),7.66(1H,d,J 8.4),8.90(1H,s)。
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