반응 #830513

ord-63bfb1918f64483d82f5a7b573156ba2

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축At the end of this time, the solution was concentrated by distillation under reduced pressure
  2. 2
    workup.DISSOLUTIONthe resulting oil was dissolved in diethyl ether
  3. 3
    기타to stand at room temperature
  4. 4
    기타The crystals which precipitated
  5. 5
    여과were collected by filtration
  6. 6
    기타dried in vacuo

실험 절차

400 mg of 1-t-butoxycarbonyl-2-(2-{2-[4-(3-methoxyphenyl)butyl]phenoxy}ethyl)piperidine [prepared as described in step (a) above] were dissolved in 2 ml of dioxane, and 2 ml of a 4N solution of hydrogen chloride in dioxane were added to the solution, which was then allowed to stand at room temperature for 30 minutes. At the end of this time, the solution was concentrated by distillation under reduced pressure, and the resulting oil was dissolved in diethyl ether and allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 276 mg (yield 80%) of the title compound as a colorless solid, melting at 76°-79° C.

출처

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