157634-02-1 1-Boc-2-哌啶甲醛

危险性质：非危险化学品

化学合成。

化学合成

合成路线 1（1. 合成：157634-02-1）

产率：94% 合成条件：With dimethyl sulfoxide; 1-hydroxy-3H-benz[d][1,2]iodoxole-1,3-dione In ethyl acetateInert atmosphere 实验步骤：合成例19; N-取代苯胺中间体XII的合成;将购买的N-Boc-2-哌啶甲醇（1.4g，1eq。）溶解在乙酸乙酯（50mL）中，并加入2-碘代苯甲酸（3.4g，1.1eq。）。将所得浆液在惰性气氛下搅拌并通过注射器加入DMSO（781μL，2.2当量）并将反应物搅拌过夜。过滤除去固体物质，滤液用10％NaS2O3 /饱和NaHCO3（1：1,3×20mL），水（1.x.20mL）和盐水（1.x.20mL）洗涤。然后真空除去有机层，得到1.3g醛（94％收率）。然后通过将醛（1.1g，1eq。）和4-氟苯胺（481μL，1eq。）溶解在二氯乙烷（20mL）中来实现偶联。在惰性气氛下，加入NaBH（OAc）3（1.5g，1.4当量）和浓乙酸（294μL，1当量），并通过TLC和LC-MS监测反应。将混合物用乙酸乙酯稀释，用10％柠檬酸（.x.3），盐水（x1）洗涤，用硫酸镁干燥。过滤混合物，通过旋转蒸发除去溶剂，真空干燥，得到1.4g中间体XII仲苯胺（90％收率）。 ESI-MS m / z = 309.1 [M + H] +。 参考文献：

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