301673-14-3 N-Boc-4-碘哌啶

危险性质：非危险化学品

化学合成；生命科学。

医药; 生命科学

合成路线 1（1. 合成：301673-14-3）

产率：93% 合成条件：With 1H-imidazole; iodine; triphenylphosphine In dichloromethane at 0 - 20℃; for 18 h; 实验步骤：向N-Boc-4-羟基哌啶（10.0g，49.7mmol）的二氯甲烷（200mL）溶液中加入三苯基膦（16.9g，64.6mmol）和咪唑（5.07g，74.5mmol）。 将所得浆液在冰浴中冷却至0℃。 分小份加入碘（15.1g，59.6mmol）。 然后将溶液在环境温度下搅拌18小时。 然后，将溶液用水稀释并用乙醚萃取。 用水和饱和NaCl水溶液洗涤有机层，然后用硫酸钠干燥。 真空浓缩，然后用己烷研磨，除去过量的三苯基膦和三苯基氧化膦。 将滤液真空浓缩，得到碘代中间体，为无色油状物（14.4g，收率93％）。 参考文献：

• [1] Patent: US2005/9838, 2005, A1. Location in patent: Page 143 [2] Patent: WO2018/106636, 2018, A1. Location in patent: Paragraph 00283 [3] Patent: WO2011/143366, 2011, A1. Location in patent: Page/Page column 45 [4] Journal of Organic Chemistry, 2004, vol. 69, # 15, p. 5120 - 5123 [5] Synlett, 1998, # 4, p. 379 - 380 [6] Patent: WO2008/147831, 2008, A1. Location in patent: Page/Page column 46 [7] Angewandte Chemie - International Edition, 2013, vol. 52, # 47, p. 12409 - 12413 [8] Angew. Chem., 2013, vol. 125, # 47, p. 12635 - 12639,5 [9] Patent: US2006/52398, 2006, A1. Location in patent: Page/Page column 62 [10] Patent: WO2013/64919, 2013, A1. Location in patent: Page/Page column 30; 31 [11] Journal of the American Chemical Society, 2018, vol. 140, # 1, p. 155 - 158 [12] Organic Letters, 2014, vol. 16, # 23, p. 6160 - 6163 [13] Chemistry - A European Journal, 2015, vol. 21, # 36, p. 12797 - 12803 [14] Bioorganic and Medicinal Chemistry Letters, 2009, vol. 19, # 5, p. 1517 - 1521 [15] Patent: WO2010/54279, 2010, A1. Location in patent: Page/Page column 127 [16] Patent: WO2011/143495, 2011, A1. Location in patent: Page/Page column 90-91 [17] Angewandte Chemie - International Edition, 2013, vol. 52, # 3, p. 933 - 937 [18] Angew. Chem., 2012, vol. 125, # 3, p. 967 - 971,5 [19] Patent: WO2015/84606, 2015, A1. Location in patent: Page/Page column 95; 96 [20] Patent: CN103130708, 2016, B. Location in patent: Paragraph 0015; 0017 [21] Organic Letters, 2017, vol. 19, # 23, p. 6412 - 6415 [22] Organic Letters, 2018, vol. 20, # 15, p. 4677 - 4680