路线1:以丙烯酰叠氮化物和苯甲醇为原料合成O-苄基-N-乙烯基氨基甲酸酯
- 原料:苯甲醇(76.5毫升,792毫摩尔)、氢醌(3.05克,27.7毫摩尔)、吡啶(3毫升,27.7毫摩尔)、1-氮杂-1-二氮杂-1,3-二烯-2-酮的甲苯溶液(200毫升)
- 步骤:向500毫升单颈烧瓶中加入苯甲醇、氢醌和吡啶,在100℃下搅拌;缓慢滴加1-氮杂-1-二氮杂-1,3-二烯-2-酮的甲苯溶液;滴加完毕后在110℃下搅拌30分钟,再室温搅拌12小时;减压蒸馏(0.4mmHg)浓缩反应混合物得粗产物,进一步纯化得到目标产物
- 产率:45%(43.1克)
- 产物性状:无色油状物(沸点110-115℃),室温静置后固化;电子喷雾质谱确认分子量为178(M*+H)
- 参考文献:
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