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2.6 反应时间对化合物Ⅱ收率的影响 1 HNMR 和 HRMS 对目标化合物进行结构表征,最
按 1.3 节方法,考察了反应时间对化合物Ⅱ收 佳工艺条件为:n(N,N-二甲基苯胺)∶n(PCl 3 )∶
率的影响,结果见表 7,当反应时间为 8 h 时,化合 n(吡啶)=1∶3∶3,110 ℃反应 24 h,化合物Ⅰ的
物Ⅱ收率为 71.4%,随着反应时间延长,化合物Ⅱ 收率达到 85.3%;n(化合物Ⅰ)∶n(CuI)∶n(LiBr)∶
收率持续增加,当反应 12 h 时,收率达到最高 n(叔丁基氯化镁)=1∶0.1∶0.2∶3,40 ℃反应 12 h,
83.4%,持续增加反应时间,化合物Ⅱ收率保持不变。 化合物Ⅱ收率可达 83.4%。
所以,最终选择最优反应时间为 12 h。 该路线避免了传统工艺中易燃的二叔丁基磷的
使用,反应过程更易控制,这对于该类配体在催化
表 7 反应时间对化合物Ⅱ收率的影响
Table 7 Effects of reaction time on the yield of compound Ⅱ 领域的进一步的应用具有很好的促进作用。
反应时间/h 参考文献:
8 10 11 12 13 14
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