反応 #1869198

ord-921de28713984b36864e4ef621b2a860

反応方程式

O=c1ccc2ccccc2[nH]1
quinolinone
CN(C)C=O
DMF
BrP(Br)Br
phosphorus tribromide
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
Brc1ccnc2ccc3c(c12)OCCO3
solid
Brc1ccnc2ccc3c(c12)OCCO3
10-Bromo-2,3-dihydro-[1,4]dioxino[2,3-f]quinoline

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooling for 30 minutes
  2. 2
    workup.STIRRINGstirred for a further 2 hours
  3. 3
    温度It was cooled in ice
  4. 4
    その他the solid was collected
  5. 5
    洗浄washed well with water
  6. 6
    その他dried in vacuo

実験手順

The quinolinone (4d) in dry DMF (8 mL) was cooled in ice and phosphorus tribromide (0.7 mL) added drop-wise, and the mixture was stirred, with ice-cooling for 30 minutes then allowed to warm to room temperature and stirred for a further 2 hours. It was cooled in ice and sodium carbonate solution was added and the solid was collected, washed well with water, and dried in vacuo, to afford a pale yellow solid (1.65 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07498326B2uspto-grants-2009_03