化学合成,医药喹那普利中间体。
医药
合成路线 1(1. 合成:74163-81-8)
产率:89%
合成条件:at 40 - 80℃; for 3 h;
实验步骤:该程序改编自文献。 将1(苯基丙氨酸)(2.0g,12.12mmol)在HBr(10mL)中的溶液加热至40℃。 然后滴加甲醛(1.8mL,48.86mmol)。 将反应混合物进一步加热至70-80℃3小时(小时),在此期间形成白色沉淀。 冷却反应,真空过滤沉淀物并用冷乙醇洗涤。 将白色固体产物置于真空下干燥。 产率= 89%(1.78g),熔点= 295-300℃(分解); 1H NMR(MeOD)δ/ ppm = 3.10(q,J = 11.41,17.23Hz,1H),3.35(dd,J = 5.28,17.20Hz,1H),4.34(dd,J = 5.38,11.47Hz,1H) ,4.37(s,2H),7.14(m,4H); 13C NMR(MeOD)δ/ ppm = 29.59,45.60,55.45,127.74,128.60,128.72,129.30,130.14,131.61,170.95; LC-MS m / z = 178.08 [M + 1],C 10 H 11 NO 2。
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