化学合成。
化学合成
合成路线 1(1. 合成:13573-28-9)
产率:76%
合成条件:With potassium hydroxide In ethanol for 90 h; Reflux
实验步骤:2.2 N-甲苯磺酰基-2-氧杂-6-氮杂螺[3.3]庚烷(5)的制备向KOH(179g,3.2mol)和对甲苯磺酰胺(205g,1.2mol)在1500mL乙醇中的溶液中加入3 在室温下加入溴-2,2-双(溴甲基)丙-1-醇(324g,1.0mol),将反应混合物加热回流90小时。 蒸发除去溶剂,加入2000mL 1M KOH,将白色悬浮液在室温下再搅拌2小时。 过滤混合物,用水冲洗白色滤饼直至洗涤水为中性。 将滤饼在高真空下干燥,得到N-甲苯磺酰基-2-氧杂-6-氮杂螺[3.3]庚烷(5,192g,产率76%),为白色固体。 1 H NMR(400MHz,CDCl 3):δ7.69(d,2H,J = 8.4Hz),7.47(d,2H,J = 8.4Hz),4.42(s,4H),3.85(s,4H),2.41( s,3H); 13 C NMR(100MHz,CDCl 3)δ144.4,130.9,130.2,128.5,79.1,59.5,37.3,21.3。
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