반응 #652850

ord-907fbaa4b6c14158945b3e77b1864ad1

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed under nitrogen gas for 3 hours
  2. 2
    추출extracted with 2 portions of ethyl acetate
  3. 3
    세척The pooled organic layer was washed with water and saturated aqueous NaCl
  4. 4
    건조dried over MgSO4
  5. 5
    여과filtered
  6. 6
    농축concentrated under reduced pressure
  7. 7
    기타The residue was crystallized from ethyl acetate/diisopropyl ether

실험 절차

A suspension of 2-bromomethyl-2,3-dihydro-2,4,6,7-tetramethyl-5-benzofuranamine (2.0 g) and potassium phthalimide (2.2 g) in N,N-dimethylacetamide (20 mL) was refluxed under nitrogen gas for 3 hours. This reaction mixture was diluted with water and extracted with 2 portions of ethyl acetate. The pooled organic layer was washed with water and saturated aqueous NaCl, dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was crystallized from ethyl acetate/diisopropyl ether to provide 1.4 g of the title compound. Yield 56%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06172085B2uspto-grants-2001_01