反应 #65159

ord-e37be0e885d140fa8bbeac76e7a1f573

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the precipitate is filtered off
  2. 2
    浓缩the filtrate is concentrated
  3. 3
    其他chromatographed on silica gel (eluent

实验过程

Sodium methylate (5.9 g) is added in portions to a solution of 1-methylpiperidine-4-thiol (14 g) in anhydrous tetrahydrofuran (100 ml) at room temperature. After 2 hours at this temperature, chloroacetone (8.8 ml) is added dropwise. After 24 hours, the precipitate is filtered off and the filtrate is concentrated and chromatographed on silica gel (eluent: ethyl acetate, then ethanol) to give 1-methyl-4-[(2-oxopropyl)thio]piperidine (11.5 g) in the form of an oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05418242uspto-grants-1995_05