반응 #830472

ord-9c0b8e648fec434397aec6ee17ab1fa5

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타At the end of this time, the solvent was removed by distillation under reduced pressure
  2. 2
    workup.DISSOLUTIONthe resulting solid residue was dissolved in a small amount of methylene chloride
  3. 3
    workup.ADDITION20 ml of ethyl acetate was then added to the solution
  4. 4
    기타thus obtained
  5. 5
    기타to stand at room temperature
  6. 6
    기타The crystals which precipitated
  7. 7
    여과were collected by filtration

실험 절차

5 ml of a 4N solution of hydrogen chloride in dioxane were added to a solution of 440 mg of 1-t-butoxycarbonyl-2-{2-[2-(2-phenylethyl)phenoxy]ethyl}piperidine [prepared as described in step (a) above] in 5 ml of dioxane, and the resulting mixture was allowed to stand at room temperature for 2 hours. At the end of this time, the solvent was removed by distillation under reduced pressure, and the resulting solid residue was dissolved in a small amount of methylene chloride; 20 ml of ethyl acetate was then added to the solution thus obtained, after which it was allowed to stand at room temperature. The crystals which precipitated were collected by filtration, to give 214 mg (yield 53%) of the title compound as colorless crystals, melting at 95°-97° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05556864uspto-grants-1996_09