반응 #622982

ord-e635d1405d3a4204bca3c56d14d26811

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After completion, the solvent was evaporated
  2. 2
    기타residue was triturated with Et2O (15 mL)
  3. 3
    기타to give crude salt
  4. 4
    추출extracted with EtOAc (3×100 mL)
  5. 5
    세척The combined extracts were washed with water (50 mL), brine (50 mL)
  6. 6
    건조dried over anhydrous Na2SO4
  7. 7
    여과filtered
  8. 8
    기타evaporated

실험 절차

To a solution of tert-butyl(trans)-2-(4-(4-bromobenzyloxy)phenyl)cyclopropylcarbamate (11 g, 26.37 mmol) in dioxane (110 mL) at 0° C., HCl in Dioxane (110 mL) was added and stirred for 1 h. After completion, the solvent was evaporated and residue was triturated with Et2O (15 mL) to give crude salt. The crude salt was dissolved in water (150 mL), basified with Na2CO3 solution, extracted with EtOAc (3×100 mL). The combined extracts were washed with water (50 mL), brine (50 mL), dried over anhydrous Na2SO4, filtered and evaporated to get (8.2 g, 98%) (trans)-2-(4-(4-bromobenzyloxy)phenyl)cyclopropanamine

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08859555B2uspto-grants-2014_10