1-氰基-环丙基羧酸乙酯是有机合成中间体和医药中间体,可用于实验室研发中有机合成过程和化工医药合成过程中。
有机合成; 医药
合成路线 1(1. 合成:1558-81-2)
产率:72%
合成条件:With tetrabutylammomium bromide; potassium carbonate In N,N-dimethyl-formamide at 80℃;
实验步骤:将氰基 - 乙酸乙酯(11.3g,0.1mol),1,2-二溴乙烷,Na 4(n-Bu)4Br和K 2 CO 3在DMF(100mL)中的悬浮液加热至80℃过夜。 将混合物倒入水(600mL)中并用EtOAc(3×50mL)萃取。 将合并的有机层用盐水洗涤,用Na 2 SO 4干燥,在减压下浓缩,得到粗产物,将其通过硅胶柱色谱纯化(石油醚:EtOAc = 10:15:1),得到1-氰基 - 环丙烷羧酸乙酯(10g,收率:72%)。 1H NMR(CDCl3 400MHz):δ4.21(q,J = 7.2Hz,2H),1.65-1.61(m,2H),1.58-1.55(m,2H),1.28(t,J = 7.2Hz,3H))
参考文献:
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合成路线 2(2. 合成:1558-81-2)
产率:59.6%
合成条件:With potassium carbonate In N,N-dimethyl-formamide at 80℃;
实验步骤:向搅拌的化合物CXI-5(30g,0.265mol),1-溴-2-氯乙烷(75g,0.528mol)的DMF(200mL)混合物中加入K 2 CO 3(110g,0.8mol)。 将反应混合物加热至80℃过夜。 将混合物用冰水稀释,用己烷萃取,用水和盐水洗涤,经Na 2 SO 4干燥,过滤并浓缩。 残余物为主要化合物CXI-6(22g,产率59.6%)并直接使用。
参考文献:
- [1] Patent: WO2013/25733, 2013, A1. Location in patent: Paragraph 0793