主要用于医药领域相关合成反应,作为中间体或原料参与特定药物合成过程。
医药
合成路线 1(1. 合成:13139-28-1)
产率:98%
合成条件:Stage #1: With N-ethyl-N,N-diisopropylamine; HATU In N,N-dimethyl-formamide at 0℃; for 0.25 h; Stage #2: With ammonium chloride In N,N-dimethyl-formamide at 23℃; for 16 h;
实验步骤:向化合物I(10g,39.84mmol,1当量)在DMF(100mL)中的填充溶液中加入DIPEA(19.7mL,119.5mmol,3当量)和HATU(18.17g,47.8mmol,1.2当量)。 )在0℃下,将所得混合物塞入15mm。向混合物中加入氯化铵(10.7g,199.2mmol,5当量),并将所得混合物在23℃下再搅拌16小时。将混合物倒入冰冷的水(500mL)中,有机组分用EtOAc(3×500mL)萃取,合并的有机层用氯化铵水溶液和盐水洗涤。将有机层用无水硫酸钠干燥,过滤并浓缩至干。粗产物用乙醇重结晶,得到标题化合物(9.8g,98%),为灰白色固体。 1H NMR(400MHz,DMSO-d6)ö7.35(m,6H),7.12(d,1H,J = 9Hz),7.01(s,1H),5.03(s,2H),3.80(t,1H, J = 8Hz),1.95(m,1H),0.85(m,6H)。 LCMS:m / z = 251.2 [M + H],RT = 2.81分钟,(程序P1,Y列)。
参考文献:
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