化学合成。
有机合成; 医药
合成路线 1(1. 合成:51529-96-5)
产率:73%
合成条件:Stage #1: at -5 - 10℃; for 1 h; Stage #2: With ammonium hydroxide In water
实验步骤:步骤1:将4-乙基-3-硝基苯胺-4-乙基苯胺(10.3mL,82.5mmol)滴加到硫酸(96%,63mL)中,冷却至8℃,保持温度低于10℃。 添加后,将反应混合物冷却至-5℃,然后加入硝酸(100%,4mL)和硫酸(96%,10mL)的混合物,保持温度低于0℃。 然后将反应混合物在相同温度下搅拌1小时。 将反应混合物倒入冰(200mL)中,过滤沉淀物并用水洗涤。 将固体用水(100mL)悬浮并用氢氧化铵(35%)中和。 过滤沉淀物并在烘箱中干燥,得到浅棕色固体(10g,73%)。1 H NMR(400MHz,DMSO-d6)δppm1.11(t,J = 7.45Hz,3H),2.63( q,J = 7.45 Hz,2 H),5.53(s,2 H),6.81(dd,J = 8.30,2.44 Hz,1 H),7.04(d,J = 2.44 Hz,1 H),7.11(d ,J = 8.30 Hz,1 H)
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