반응 #163545

ord-cffd98ecd0f34ad1a0c86bed52615424

반응 방정식

O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
CCn1c(=O)c(=O)[nH]c2ccccc21
1-ethyl-1,4-dihydroquinoxaline-2,3-dione
O=P(Br)(Br)Br
POBr3
CCn1c(=O)c(Br)nc2ccccc21
3-bromo-1-ethyl-quinoxalin-2(1H)-one
수율 53.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was refluxed
  2. 2
    workup.ADDITIONtreated with ice cold
  3. 3
    여과The mixture was filtered
  4. 4
    추출the filtrate was extracted with dichloromethane
  5. 5
    건조dried over anhydrous sodium sulfate
  6. 6
    농축concentrated

실험 절차

To 2 g (10.5 mM) of 1-ethyl-1,4-dihydroquinoxaline-2,3-dione in 20 ml of dichloroethane were added dropwise 3.16 g (11.0 mM) of POBr3. The reaction mixture was refluxed under stirring for 2 h and then treated with ice cold and an aqueous sodium carbonate solution. The mixture was filtered and the filtrate was extracted with dichloromethane, dried over anhydrous sodium sulfate and concentrated to give 1.4 g of 3-bromo-1-ethyl-quinoxalin-2(1H)-one as a yellow solid. Yield: 53%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08835634B2uspto-grants-2014_09