化学合成。
医药
合成路线 1(1. 合成:23680-40-2)
产率:98%
合成条件:With N-Bromosuccinimide; silver nitrate In acetone at 20 - 32℃;
实验步骤:向溶解在丙酮(2L)中的丙炔酸甲酯(60g,713.6mmol)中加入N-溴代琥珀酰亚胺(147.22g,827.13mmol),然后加入硝酸银(12.12g,71.37mmol)。 观察到轻微的放热,反应温度从21-32℃升高,然后将反应混合物在室温下搅拌过夜。 将得到的灰色悬浮液真空蒸发至干,加入戊烷(100mL)并通过Celite过滤,用更多的戊烷洗涤。 该过程再进行两次,然后将合并的滤液真空蒸发,得到113g 3-溴丙醇甲酯(98%收率),含有约10%的原料.1 H NMR(400MHz,CDCl 3)δppm3.78(s, 3 H)。
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