반응 #1605795

ord-5716d326ab464fea9688467c459fe100

반응 방정식

CC(=O)c1ccc(O)c2[nH]c(=O)ccc12
5-Acetyl-8-hydroxy-1H-quinolin-2-one
O=C([O-])[O-].[K+].[K+]
potassium carbonate
BrCc1ccccc1
benzyl bromide
CC(=O)c1ccc(OCc2ccccc2)c2[nH]c(=O)ccc12
5-acetyl-8-benzyloxy-1H-quinolin-2-one
수율 87.4%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The insoluble matter was removed by filtration
  2. 2
    세척washed with N,N-dimethylformamide
  3. 3
    workup.ADDITIONThe filtrate and the washing were mixed
  4. 4
    농축concentrated under reduced pressure
  5. 5
    workup.ADDITIONTo the residue was added
  6. 6
    기타purified water (3.3 L)
  7. 7
    workup.STIRRINGthe mixture was stirred at room temperature overnight
  8. 8
    여과The precipitate was collected by filtration
  9. 9
    세척washed with purified water
  10. 10
    기타dried under vacuum

실험 절차

5-Acetyl-8-hydroxy-1H-quinolin-2-one (430 g, 2.12 mol) was suspended in N,N-dimethylformamide (3.3 L), potassium carbonate (298 g, 2.16 mol) and subsequently benzyl bromide (298 g, 2.11 mol) were added thereto, and the mixture was stirred at room temperature for 2 hours. The insoluble matter was removed by filtration and washed with N,N-dimethylformamide. The filtrate and the washing were mixed and concentrated under reduced pressure. To the residue was added purified water (3.3 L) and the mixture was stirred at room temperature overnight. The precipitate was collected by filtration, washed with purified water, and dried under vacuum to obtain 5-acetyl-8-benzyloxy-1H-quinolin-2-one (541 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09072734B2uspto-grants-2015_07