반응 #170046

ord-91ba1bcecf0941e2b78d44b8d9e8c6a6

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISSOLUTIONthe solid gradually dissolved
  2. 2
    세척by washing it with brine (1×50 mL)
  3. 3
    기타The organic phase was collected
  4. 4
    기타dried on MgSO4
  5. 5
    기타evaporated
  6. 6
    기타The residue was purified by flash-chromatography on silica gel (100% DCM)

실험 절차

tert-Butyl 7-(aminomethyl)-1-benzyl-1,2,3,4-tetrahydronaphthalen-2-ylcarbamate (0.600 g, 1.637 mmol) was suspended in dichloromethane (5 mL) and triethylamine (0.228 mL, 1.637 mmol) and cooled to 0° C. Ethanesulfonyl chloride (0.155 mL, 1.64 mmol) was added and the solid gradually dissolved. After 30 minutes the reaction was stopped by washing it with brine (1×50 mL). The organic phase was collected and dried on MgSO4, evaporated. The residue was purified by flash-chromatography on silica gel (100% DCM). Product was obtained as yellow solid (0.653 g, 1.42 mmol, 87%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846741B2uspto-grants-2014_09