化学合成;以1-甲基-1H-吲哚-5-氯为起始物料经氨解反应制备;或以1-甲基-1H-吲哚-5-硝基为起始物料经加氢还原(雷尼镍为催化剂)制备;或以5-硝基吲哚为起始物料经与碘甲烷反应制备1-甲基-1H-吲哚-5-硝基后再经硝基还原制得。
化学合成
合成路线 1(1. 合成:102308-97-4)
- 步骤:将10%Pd / C(0.18g / g起始材料)加入到溶解在THF中的原料溶液(54mL / g原料)中;密封反应烧瓶并使用真空除去空气;将充满氢气的气球连接到烧瓶上;将反应在室温下搅拌24小时至48小时或直至通过TLC观察到起始材料的消失;将反应物通过硅藻土过滤;将滤液旋转蒸发,得到棕色固体。
- 条件:With palladium 10% on activated carbon; hydrogen In tetrahydrofuran at 20℃。
- 收率:100%。
- 表征数据:1H NMR(DMSO):δ7.15-7.05(m,2H),6.71(dd,J 3.0,0.9Hz,1H),6.57(dd,J 8.5,2.1Hz,1H),6.12(dd,J 3.0,0.9Hz,1H),3.67(s,3H);13CNMR(DMSO):δ141.30,131.12,129.49,129.44,129.41,112.31,110.11,104.21,99.13,32.86。
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