反应 #2325

ord-b74bffc65057435d9d7a9739ada92f3c

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他hydrogenated at room temperature
  2. 2
    过滤then filtered through diatomaceous earth
  3. 3
    其他the filtrate evaporated to dryness

实验过程

10% w/w Palladium on charcoal (1.5 g) was added to a solution of the product from step (i) (10.0 g), 1 molar hydrochloric acid (21.5 ml) and methanol (150 ml) and the mixture hydrogenated at room temperature and pressure until the theoretical amount of hydrogen had been taken up. Charcoal was added, the mixture stirred for 1 hour then filtered through diatomaceous earth and the filtrate evaporated to dryness giving 4-acetylaminopiperidine hydrochloride, 8.64 g, as a sticky foam: NMR (CDCl3 +d6DMSO). δ 9,72(1H,b), 9.02(1H,b), 7.40(1H,bd), 3.87(1H,m), 3.30(2H,m), 2.81(2H,m), 1.86(4H,m), 1.80(3H,s); m/e 143 (M+H)+.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05728701uspto-grants-1998_03