反応 #417948

ord-9d2bb70262ba419b9dad22782050253a

反応方程式

Oc1ccc(Br)nc1
2-bromo-5-hydroxypyridine
CCCBr
1-bromopropane
O=C([O-])[O-].[K+].[K+]
K2CO3
CCCOc1ccc(Br)nc1
2-Bromo-5-propoxy-pyridine

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度at reflux over night
  2. 2
    その他Afterwards the reaction is quenched by the addition of water
  3. 3
    抽出extracted with TBME
  4. 4
    乾燥dried over MgSO4
  5. 5
    ろ過filtered
  6. 6
    その他the solvent is removed in vacuo
  7. 7
    その他The crude product is purified by column chromatography (silica gel, PE/EtOAc)

実験手順

10.0 g (57.5 mmol) 2-bromo-5-hydroxypyridine, 28.3 g (230 mmol) 1-bromopropane and 19.9 g (143.7 mmol) K2CO3 are added to 1 L ACN and stirred at reflux over night. Afterwards the reaction is quenched by the addition of water and extracted with TBME. The org. layers are combined, dried over MgSO4, filtered and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel, PE/EtOAc).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08877741B2uspto-grants-2014_11