21075-83-2 1-甲基-1-叔丁氧羰基肼

危险性质：非危险化学品

化学合成。

医药

合成路线 1（1. 合成：21075-83-2）

产率：97% 合成条件：With sodium hydroxide In methanol at 0 - 20℃; for 4 h; 实验步骤：将甲基肼（7）（26g，564mmol）和氢氧化钠（23g，575mmol）溶解在甲醇（500mL）中。 在0℃下，在2小时内向该溶液中滴加二碳酸二叔丁酯（123g，564mmol）的甲醇（500mL）溶液。将反应溶液在室温下搅拌2小时，沉积物 通过硅藻土过滤除去，滤液真空蒸发。 加入油状残余物，用氯化铵水溶液中和。用二氯甲烷萃取溶液，用MgSO 4干燥，然后蒸发，得到标题化合物8（79g，97％）。1H NMR（CDCl3）d：4.06（br， 2H），3.05（s，3H），1.47（s，9H）; IR（纯）1694,1365,1154 cm1。 参考文献：

• [1] Bioorganic and Medicinal Chemistry Letters, 2003, vol. 13, # 14, p. 2413 - 2418 [2] Chirality, 2013, vol. 25, # 6, p. 341 - 349 [3] Journal of Antibiotics, 1993, vol. 46, # 8, p. 1279 - 1288 [4] Patent: US5275816, 1994, A [5] Bioorganic Chemistry, 2010, vol. 38, # 5, p. 229 - 233 [6] Bioorganic and Medicinal Chemistry, 2014, vol. 22, # 15, p. 4162 - 4176 [7] Patent: US2007/49632, 2007, A1. Location in patent: Page/Page column 11 [8] Patent: US2005/256107, 2005, A1. Location in patent: Page/Page column 53 [9] Chemische Berichte, 1982, vol. 115, # 8, p. 2807 - 2818 [10] Journal of Heterocyclic Chemistry, 2000, vol. 37, # 1, p. 47 - 55 [11] Patent: CN108178740, 2018, A. Location in patent: Paragraph 0033; 0034 [12] ChemMedChem, 2013, vol. 8, # 8, p. 1314 - 1321 [13] The Journal of organic chemistry, 2002, vol. 67, # 25, p. 8962 - 8969 [14] Organic Letters, 2015, vol. 17, # 2, p. 254 - 257 [15] ACS Medicinal Chemistry Letters, 2014, vol. 5, # 10, p. 1076 - 1081 [16] Patent: US6413997, 2002, B1 [17] Patent: US6015826, 2000, A [18] Chemical Communications, 2012, vol. 48, # 46, p. 5772 - 5774 [19] Journal of Organic Chemistry, 1999, vol. 64, # 1, p. 276 - 281 [20] Journal of Organic Chemistry, 2005, vol. 70, # 26, p. 10701 - 10708 [21] Patent: US4904775, 1990, A [22] Patent: US5030724, 1991, A [23] Patent: US5112968, 1992, A [24] Journal of Medicinal Chemistry, 2008, vol. 51, # 4, p. 924 - 931 [25] Patent: WO2005/87764, 2005, A1. Location in patent: Page/Page column 26 [26] Bioorganic and Medicinal Chemistry, 2015, vol. 23, # 15, p. 4952 - 4969 [27] Journal of Medicinal Chemistry, 2016, vol. 59, # 12, p. 5799 - 5809 [28] Patent: WO2005/123717, 2005, A1. Location in patent: Page/Page column 16; 18