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·1794·                            精细化工   FINE CHEMICALS                                  第 35 卷

            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。
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                        8     10    11    12    13    14
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