반응 #80667

ord-11a9fe98919548ab93c362e6c3d18f58

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThe mixture is subsequently poured onto ice
  2. 2
    추출extracted with diethyl ether
  3. 3
    건조After the diethyl ether solution has been dried over sodium sulfate
  4. 4
    기타the ether is evaporated
  5. 5
    workup.DISSOLUTIONthe viscous residue is dissolved in 300 ml of warm acetonitrile
  6. 6
    여과The solution is filtered
  7. 7
    기타to crystallize

실험 절차

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%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05616637uspto-grants-1997_04