24214-72-0
24214-72-0 结构式
基本信息
环戊基-肼 盐酸盐
环戊肼盐酸盐(CAS号:24214-72-0)
1-CYCLOPENTYLHYDRAZINE HCL
cyclopentylhydrazine, HCl salt
cyclopentyl-hydrazinhydrochloride
Hydrazinocyclopentane hydrochloride
CYCLOPENTYL HYDRAZINE HYDROCHLORIDE
1-CYCLOPENTYHYDRAZINE HYDROCHLORIDE
CYCLOPENTYLHYDRAZINE
HYDRON
CHLORIDE
1-CYCLOPENTYLHYDRAZINE HYDROCHLORIDE
物理化学性质
制备方法
79201-39-1
24214-72-0
步骤2:环戊肼盐酸盐的合成 将N'-环戊基亚基肼甲酸叔丁酯(5.448 g,27.48 mmol)溶于无水四氢呋喃(25 mL)和无水甲醇(34 mL)的混合溶剂中。在氩气保护下,分批加入氰基硼氢化钠(2.044 g,32.53 mmol),随后将反应混合物回流10分钟。反应完成后,冷却至室温,加入6N盐酸(12 mL),继续回流1.5小时。通过NMR分析等分试样,确认仍有部分BOC保护基未脱除。补加6N盐酸,继续回流3小时。反应结束后,冷却至室温并搅拌过夜。过滤除去不溶物,滤液经浓缩后与甲苯共沸三次以彻底除去水分。将残余物溶解于热异丙醇中,冷却至室温后,用乙醚稀释并进一步冷却。过滤收集固体,得到环戊肼盐酸盐(3.903 g,产率103%),该产物无需进一步纯化即可用于后续反应。
参考文献:
[1] Patent: US2007/225280, 2007, A1. Location in patent: Page/Page column 48
[2] Patent: WO2014/16789, 2014, A1. Location in patent: Page/Page column 18; 19
[3] Bioorganic and Medicinal Chemistry, 2004, vol. 12, # 2, p. 393 - 404
[4] Journal of Organic Chemistry, 1981, vol. 46, # 26, p. 5413 - 5414
[5] Patent: US2004/220186, 2004, A1. Location in patent: Page 19
