Diethyl Ether → Ethyl (6-bromo-2-nitropyridin-3-yloxy)acetate

HRID 639053ノート

反応式

HRID 639053 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([N+:9]([O-:11])=[O:10])[N:3]=1.C(=O)([O-])[O-:13].[K+].[K+].[CH3:18][CH2:19][O:20][CH2:21][CH3:22]>CC(C)=O.BrCC(OCC)=O>[CH2:19]([O:20][C:21](=[O:13])[CH2:22][O:8][C:5]1[C:4]([N+:9]([O-:11])=[O:10])=[N:3][C:2]([Br:1])=[CH:7][CH:6]=1)[CH3:18]

参加物

6

反応物 3

HCID 3283Diethyl EtherHCID 11430Potassium CarbonateHCID 218738086-Bromo-2-nitropyridin-3-ol

生成物 1

HCID 59560649Ethyl (6-bromo-2-nitropyridin-3-yloxy)acetate収率 89%

試薬・触媒・溶媒 2

HCID 7748Ethyl bromoacetate触媒HCID 180Acetone溶媒

実験手順

2-Bromo-5-hydroxy-6-nitropyridine (30 g, 0.14 mole) was suspended in acetone (200 ml), and potassium carbonate (39 g, 0.28 mole) was added, followed by ethyl bromoacetate (15.7 ml, 0.14 mmole). The reaction was heated at reflux for 10 hr, 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; MS (ES) m/z 305.0 (M+H)+.

後処理

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 10 hr
  3. customThe precipitate was removed by suction filtration
  4. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-d3e7e008c76d4b32a256040140b882b0
出典データセット
uspto-grants-2010_04
特許番号
US07691850B2

反応ノート

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