用于后续反应(具体应用领域未明确说明,基于专利和文献推测可能用于医药或农药相关合成)
医药; 农药
合成路线 1(1. 合成:99419-31-5)
产率:71%
合成条件:With trichloroisocyanuric acid In dichloromethane at -5 - 20℃; for 0.67 h;
实验步骤:制备193-将甲基氧杂环丁烷-3-甲醛(3-甲基氧杂环丁烷-3-基)甲醇(6.0g,58.75mmol)溶解在二氯甲烷(117mL)中。 在-5℃下分批加入三氯异氰尿酸(13.93g,59.92mmol),然后加入2,2,6,6-四甲基哌啶-1-氧基(TEMPO)(0.92g,5.87mmol)。 将反应混合物在-5℃下搅拌20分钟,使其温热至室温,并再搅拌20分钟。 将混合物通过CELITE垫过滤,用二氯甲烷(200mL)稀释,并用饱和Na 2 CO 3水溶液(100mL),1N HCl(100mL)和盐水(50mL)洗涤。 浓缩有机部分,得到标题化合物,为橙色油状物(4.17g,71%),无需进一步纯化即可使用。 XH NMR(400MHz,CDCl3); δ1.48(s,3H),4.50(d,2H,J = 6.34Hz),4.88(d,2H,J = 6.34Hz),9.95(s,1H)。
参考文献:
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