反应 #80667

ord-11a9fe98919548ab93c362e6c3d18f58

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONThe mixture is subsequently poured onto ice
  2. 2
    萃取extracted with diethyl ether
  3. 3
    干燥After the diethyl ether solution has been dried over sodium sulfate
  4. 4
    其他the ether is evaporated
  5. 5
    workup.DISSOLUTIONthe viscous residue is dissolved in 300 ml of warm acetonitrile
  6. 6
    过滤The solution is filtered
  7. 7
    其他to crystallize

实验过程

24 g (428 mmol) of potassium hydroxide are dissolved in 600 ml of methanol in a conical flask. 85 g (286 mmol) of 1-cyclohexyloxy-2,2,6,6-tetramethyl-4-acetoxypiperidine are poured into the warm solution with stirring. The mixture is subsequently poured onto ice and extracted with diethyl ether. After the diethyl ether solution has been dried over sodium sulfate, the ether is evaporated and the viscous residue is dissolved in 300 ml of warm acetonitrile. The solution is filtered and allowed to crystallize; yield: 50 g (68%). The colourless substance has a melting point of 78.5° C.; purity according to GC analysis: 96%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05616637uspto-grants-1997_04