化学合成。
化学合成
合成路线 1(1. 合成:33301-41-6)
产率:100%
合成条件:With triethylamine In dichloromethane at 0℃; for 2 h;
实验步骤:甲磺酸1-二苯甲基 - 氮杂环丁烷-3-基酯(12)(方案5,步骤8)。 在氮气下,在0℃(冰 - 水浴)下,向1-二苯甲基 - 氮杂环丁烷-3-醇(15.0g,62.7mmol)的无水CH 2 Cl 2(1mL)溶液中加入干燥的Et 3 N(25mL,94.0mmol))。 然后通过加压均流加料漏斗向其中滴加甲磺酰氯(5.8mL,75.2mmol)的无水CH 2 Cl 2(50mL)溶液。 加完后,移去冷却浴,搅拌混合物2小时。 将非均相混合物用H 2 O(70mL)处理,分离各层,水层用CH 2 Cl 2(2.x.100mL)萃取。 将合并的有机萃取液干燥(MgSO 4),过滤并浓缩,得到澄清无色油状物。 加入己烷(100mL)后,粘稠的油状产物固化并通过真空过滤收集。 在高真空下干燥,得到19.7g(100%收率)12,为无色固体。
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