반응 #46724

ord-2d84f94ad95e48038928e9c8df4fb329

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONpoured onto H2O (150 mL)
  2. 2
    workup.DISSOLUTIONto dissolve any precipitated material
  3. 3
    기타The organic layer was Isolated
  4. 4
    세척washed with H2O (50 mL)
  5. 5
    건조dried (MgSO4)
  6. 6
    여과filtered
  7. 7
    기타the eluate evaporated to dryness

실험 절차

To a solution of N-(2,4-dimethoxy phenyl)-2,2,2-trifluoro-acetamide (2.50 g; 10 mmol) in CH2Cl2 (20 mL) cooled to −10° C. was added 1 M BBr3 (CH2Cl2; 24 mL; 24 mmol) under N2 atmosphere. The mixture was allowed to warm to room temperature over 2 hours and poured onto H2O (150 mL). Saturated aqueous NaHCO3 (100 mL) and diethylether (100 mL) was added to dissolve any precipitated material. The organic layer was Isolated, washed with H2O (50 mL), dried (MgSO4), filtered and the eluate evaporated to dryness to yield 1.85 g (83%) of the desired compound as a greyish solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741352B2uspto-grants-2010_06