Bromine → 6-Bromo-2-nitropyridin-3-ol

HRID 639040

反応式

HRID 639040 の反応式
[OH:1][C:2]1[C:3]([N+:8]([O-:10])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1.C[O-].[Na+].[Br:14]Br>CO>[Br:14][C:5]1[CH:6]=[CH:7][C:2]([OH:1])=[C:3]([N+:8]([O-:10])=[O:9])[N:4]=1

参加物

5

反応物 3

HCID 24408BromineHCID 270573-Hydroxy-2-nitropyridineHCID 10942334Sodium Methoxide

生成物 1

HCID 218738086-Bromo-2-nitropyridin-3-ol収率 97.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
0 °C

実験手順

3-Hydroxy-2-nitropyridine (20 g, 0.143 mole) was dissolved in methanol (400 mL) and a solution of 25% sodium methoxide in methanol (33 mL, 0.13 mole) was added at room temperature. The mixture was stirred for 30 min, then was cooled to 0° C., and bromine (7.2 mL, 0.14 mole) was added slowly. The reaction was stirred at 0° C. for 30 min, then was quenched with glacial AcOH (2.5 mL). The solvent was removed in vacuo to afford material (30 g, 96%), which was used without further purification.

後処理

  1. stirringThe reaction was stirred at 0° C. for 30 min
  2. customwas quenched with glacial AcOH (2.5 mL)
  3. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-d8ad9ed8ce5c495fbb0cb6c2cbccac62
出典データセット
uspto-grants-2010_04
特許番号
US07691850B2

関連ノート

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