反応 #1869192

ord-1771243a14b444e290dbf8af8b46e80b

反応方程式

O=[N+]([O-])c1nc(Br)ccc1O
hydroxypyridine
O=[N+]([O-])c1nc(Br)ccc1O
2-Bromo-5-hydroxy-6-nitropyridine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CCOCC
Et2O
CCOC(=O)COc1ccc(Br)nc1[N+](=O)[O-]
material
収率 89.0%
CCOC(=O)COc1ccc(Br)nc1[N+](=O)[O-]
Ethyl (6-bromo-2-nitro-pyridin-3-yloxy)acetate
収率 89.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction was heated
  2. 2
    温度at reflux for 10 hours
  3. 3
    その他The precipitate was removed by suction filtration
  4. 4
    濃縮the filtrate was concentrated in vacuo

実験手順

The hydroxypyridine (f) (30 g, 0.14 mol) was suspended in acetone (200 ml), and potassium carbonate (39 g, 0.28 mol) was added, followed by ethyl bromoacetate (15.7 ml, 0.14 mmol). The reaction was heated at reflux for 10 hours, then was cooled to room temperature and diluted with Et2O. The precipitate was removed by suction filtration, and the filtrate was concentrated in vacuo to afford material (38 g, 89%), which was used without further purification.

出典

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