化学合成。
化学合成
合成路线 1(1. 合成:15771-06-9)
产率:83%
合成条件:With sodium hydroxide In methanol; water for 18.50 h; Reflux
实验步骤:将曲酸(11)(14.20g,100mmol)溶解在甲醇(100mL)中,并加入氢氧化钠(4.40g,110mmol)的水(10mL)溶液。 将反应混合物加热至回流。 然后在30分钟内滴加苄基氯(13.92g,110mmol)并回流18小时。 浓缩反应混合物,向残余物中加入二氯甲烷(400mL)。 滤除无机盐。 用5%氢氧化钠溶液(100mL),水(100mL)洗涤二氯甲烷,用Na 2 SO 4干燥,过滤,浓缩并从乙醇中重结晶,得到浅黄色固体(12b)(19.26g,83%)。
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