作为医药合成中间体,用于有机合成反应中保护氨基基团。
医药
合成路线 1(1. 合成:137618-48-5)
产率:100%
合成条件:With sodium hydroxide In tert -butyl alcohol at 0 - 20℃; for 5 h;
实验步骤:将3g(1.0当量,32.93mmol)3-氨基-1,2-丙二醇23溶于20mL叔丁醇和20mL 1M NaOH中,并在冰冷却下,加入20mL叔丁醇溶液含有7.19克(1.0当量,32.93毫摩尔)Boc2O。之后,在室温下搅拌5小时。通过TLC确认反应物质消失后,使用蒸发器在50℃的水浴中减压浓缩。然后,使用1M HCl中和反应溶液。通过加入乙酸乙酯和水进行中和溶液的液体分馏萃取3次,并将收集的有机层用饱和NaCl水溶液洗涤。用硫酸镁干燥后,使用蒸发器在40℃的水浴中减压浓缩。结果,得到6.3g所需化合物2(产率:定量)。 1H-NMR信号分配如下:1 H-NMR(500MHz,CDCl3)δ1.45(9H,s),2.68-2.71(1H,br),2.75-2.81(1H,br),3.20(2H) ,dd),3.63(2H,dd),3.71(1H,m)4.91(1H,br)。
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