作为有机合成中间体,用于制备相关功能材料或药物分子。
医药; 材料
合成路线 1(1. 合成:1723-27-9)
产率:100%
合成条件:With lithium hydroxide monohydrate In water at 100℃; for 3 h; Inert atmosphere; Large scale
实验步骤:在氮气氛下,将氢氧化锂一水合物(17. 8Kg,662.4mol,1.47当量),H 2 O(440.0OKg)加入到2000L高压釜中并搅拌以将氢氧化锂一水合物溶解在水中。 在室温下,将中间体3(95.5?,449.8111 01,1.069)泵入反应混合物中,然后加入1'(379.5)。 加热至回流(约100℃)3小时,冷却至35至40℃并在氮气氛下通过减压旋转蒸发除去四氢呋喃将水(200Kg)加入反应容器中控制温度低于20° C(74.6Kg),过滤并将滤饼用冷水(20Kg)洗涤三次并离心直至不得到液体,产物4(146Kg,产率100%)。
参考文献:
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