表6 DPPA的用量对合成UBT的影响Tab.6 Effect of the amount of DPPA on the synthesis of UBTn(DPPA): n(中间体2) UBT的纯度/% UBT的摩尔收率/%1.2:1.0 73.33 56.16 1.3:1.0 91.87 70.39 1.4:1.0 98.78 76.58 1.5:1.0 99.50 77.50 1.6:1.0 99.52 76.97

表7 BocEDA的用量对合成UBT的影响Tab.7 Effect of the amount of BocEDA on the synthesis of UBTn(BocEDA): n(中间体2) UBT的纯度/% UBT的摩尔收率/%1.0:1.0 83.21 42.27 1.1:1.0 98.87 65.36 1.2:1.0 99.50 77.50 1.3:1.0 99.47 77.61 1.4:1.0 99.43 76.43

3 结论

本工艺首先是以1-甲基-5-氨基-4-乙氧羰基吡唑与三苯基氯甲烷为起始原料，两者进行缩合反应得到中间体1，其中三苯基氯甲烷与1-甲基-5-氨基-4-乙氧羰基吡唑的最佳摩尔比为1.3:1.0，其缚酸剂吡啶与1-甲基-5-氨基-4-乙氧羰基吡唑的最佳摩尔比为1.3:1.0；然后中间体1在氢氧化钠甲醇水溶液进行水解反应得到中间体2，其中氢氧化钠与1-甲基-5-氨基-4-乙氧羰基吡唑的最佳摩尔比为8.0:1.0，后期反应的析晶体系最佳pH值范围为(3.)；最后中间体2再与DPPA、BocEDA进行一锅法反应得到产品UBT，其中BocEDA与中间体2的最佳摩尔比为1.2:1.0。该工艺合成的UBT不仅纯度及收率比较高，而且所用原料易得，适合工业化生产。因此，此工艺路线具有较大的社会经济效益。

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