반응 #1278052

ord-9c2f6784ad24477b9389ca1675cf4541

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과filtered through a celite pad
  2. 2
    기타The filtrate was evaporated
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in DCM
  4. 4
    세척washed with an saturated aqueous solution of Na2CO3
  5. 5
    추출The aqueous layer was extracted with DCM
  6. 6
    건조The combined organic layers were dried over Na2SO4
  7. 7
    여과filtered
  8. 8
    기타evaporated

실험 절차

[2-(4-Methylpiperazin-1-yl)-5-nitrophenyl]methanol prepared in step A of example 1 (1.00 g, 3.98 mmol) was hydrogenated using ammonium formate (2.51 g, 10 eq) and Pd/C (10% Pd, 0.43 mg, 0.1 eq) in 50 mL of EtOH. The mixture was stirred overnight at room temperature and then filtered through a celite pad. The filtrate was evaporated and the residue was dissolved in DCM and washed with an saturated aqueous solution of Na2CO3. The aqueous layer was extracted with DCM. The combined organic layers were dried over Na2SO4, filtered and evaporated to yield expected compound as a pale yellow oil (0.85 g, 97% yield).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08680095B2uspto-grants-2014_03