반응 #169034

ord-f1a539272cc84c67a0729afb79c67f70

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGwith stirring
  2. 2
    workup.ADDITIONThe reaction mixture was poured into ice
  3. 3
    workup.STIRRINGstirred 35 minutes
  4. 4
    여과filtered
  5. 5
    세척The solid was washed with water
  6. 6
    추출The filtrate was extracted with EtOAc and solvent
  7. 7
    기타was removed under reduced pressure

실험 절차

N-(3-Methoxy-phenyl)-acetamide (17.7 g, 107 mmol) in methylene chloride was cooled to zero degrees C., and acetyl chloride (19.0 ml, 268 mmol) was slowly added, followed by aluminum chloride (35.7 g, 268 mmol) in small portions over 15 min. The reaction mixture was stirred 15 minutes at zero degrees, then allowed to warm to room temperature with stirring. The reaction mixture was poured into ice, stirred 35 minutes, and filtered. The solid was washed with water. The filtrate was extracted with EtOAc and solvent was removed under reduced pressure. The combined solids gave N-(4-Acetyl-3-methoxy-phenyl)-acetamide (16.5 g., 74%) as a solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846705B2uspto-grants-2014_09