化学合成。
医药
合成路线 1（2. 合成：443797-96-4）
产率：13.6 %Chromat.
合成条件：With potassium carbonate In isopropyl alcohol at 80 - 85℃; for 6 h;
实验步骤：进行一系列实验以确定溶剂和碱对HPLC测定的标题产物收率的影响。实验的一般程序如下。 N- [4-（氨基磺酰基）苯基] -N'-氰基氨基甲酸苯酯（0.5g，1.60mmol）和2,6-二氟苯甲酰肼（0.3g，1.74mmol）在15mol所选溶剂中的混合物（在加入（2.08mmol，1.3当量）所选碱的过程中搅拌（参见下表4）（参见下表4）。将反应混合物加热至约80-85℃并在该温度下保持6小时。将反应混合物冷却至约20-25℃后，取出样品用于HPLC分析。通过用乙腈和水（50/50）稀释等分试样来制备HPLC样品，以确定转化为标题化合物的百分比，结果列于下表4中。表4：溶剂和碱对标题产物收率的影响a，b溶剂MeOH THF DME IPA MeCN碱= K 2 CO 3收率3. 3 31. 0 17. 5 13. 6 3. 0碱= Cs 2 CO 3收率0.0 3.6 3.6 0.9 0.2碱= TEA产率5.0 5.4 5.5 1.1 20.7c碱= DIPEA产率1.8 2.8 1.6 2.7 16.1d碱=吡啶产率5.9 6.9 4.2 2.2 11.0碱= KOHe产率14. 5 9. 3碱= NaOH颗粒产率百分比5.0 10.0 HPLC向标题化合物的转化率b在所有情况下均观察到不同量的异脲交换产物和分解，除了那些使用吡啶c的HPLC分析显示 - 3％的另一种区域异构体d HPLC分析显示~1。 4％的另一种区域异构体e颗粒
参考文献：
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