路线1:N-Boc-(2S,3S)-3-羟基-2-羧基吡咯烷甲基化反应
- 原料:N-Boc-(2S,3S)-3-羟基-2-羧基吡咯烷(37.16 g,71 mmol)、DMF(100 mL)、K₂CO₃(16 g,116 mmol)、碘甲烷(5.4 mL,87 mmol)
- 步骤:将原料溶于DMF并冷却至0℃,加入K₂CO₃后缓慢滴加碘甲烷;1小时内升温至室温(溶液变为黄色非均相混合物);90℃加热1小时后冷却至室温;反应液用饱和盐水稀释,乙醚萃取;合并有机相,无水Na₂SO₄干燥,过滤后减压浓缩
- 产物:(2S,3S)-1-(叔丁氧基羰基)-3-羟基-吡咯烷-2-甲酸甲酯(14.8 g,黄色油状物)
- 收率:87%
- 参考文献:
[1] Patent: US2008/20986, 2008, A1. Location in patent: Page/Page column 16
[2] Patent: WO2009/94287, 2009, A1. Location in patent: Page/Page column 31
[3] Patent: WO2010/138496, 2010, A1. Location in patent: Page/Page column 38-39
[4] Patent: WO2011/68926, 2011, A1. Location in patent: Page/Page column 39-40
[5] Patent: WO2010/33531, 2010, A1. Location in patent: Page/Page column 66