23761-23-1
100-51-6
130369-36-7
以3-氧代环丁烷羧酸(1.0g,8.77mmol)和苯甲醇(1.14g,10.52mmol)为原料,在氩气保护下,将3-氧代环丁烷羧酸与DIEA(1.92g,14.92mmol)和DPPA(2.89g,10.52mmol)在甲苯(8mL)中混合。将反应混合物加热至60℃并维持3小时,随后加入苯甲醇。继续在60℃下搅拌过夜。反应完成后,浓缩反应混合物,残余物通过硅胶柱色谱法(石油醚:乙酸乙酯 = 8:1)纯化,得到目标产物3-氧代环丁基氨基甲酸苄酯(240mg,收率50%)。产物经1H NMR(500MHz,CDCl3)和ESI-MS表征:1H NMR δ 7.38-7.33(m,5H),5.12(d,J = 7.5Hz,2H),4.34-4.33(brs,1H),3.44-3.39(m,2H),3.10-3.07(brs,2H)ppm;ESI-MS(m/z):220.2 [M + 1]+。
参考文献:
[1] Patent: WO2012/75381, 2012, A1. Location in patent: Page/Page column 210
[2] Patent: WO2012/9678, 2012, A1. Location in patent: Page/Page column 210
[3] Patent: EP1256578, 2002, A1. Location in patent: Page 22
[4] Patent: WO2014/74421, 2014, A1. Location in patent: Page/Page column 56; 57