Hydrogen Bromide → 4-Bromo-2,3-dimethylpyridine 1-oxide

HRID 254253

反応式

HRID 254253 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([N+]([O-])=O)[CH:5]=[CH:4][N+:3]=1[O-:12].[BrH:13]>>[Br:13][C:6]1[CH:5]=[CH:4][N+:3]([O-:12])=[C:2]([CH3:1])[C:7]=1[CH3:8]

参加物

3

反応物 2

HCID 260Hydrogen BromideHCID 1482232,3-Dimethyl-4-nitropyridine-N-oxide

生成物 1

HCID 589974274-Bromo-2,3-dimethylpyridine 1-oxide

反応条件

温度
100 °C

実験手順

A mixture of 2,3-dimethyl-4-nitropyridine N-oxide (5 g, 29.7 mmol) and hydrogen bromide (30% wt in acetic acid, 100 mL) was heated for 48 hours at 100° C. The mixture was then filtered, washing through with 2M sodium hydroxide and the filtrate was extracted with dichloromethane (×3). The combined organic solutions were washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel, eluting with ethyl acetate:pentane, 50:50, to afford the title product as a pale yellow solid.

後処理

  1. filtrationThe mixture was then filtered
  2. washwashing through with 2M sodium hydroxide
  3. extractionthe filtrate was extracted with dichloromethane (×3)
  4. washThe combined organic solutions were washed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography on silica gel
  8. washeluting with ethyl acetate

出典と根拠

ORDレコード
ord-d418d361687d4d1393b167dbf84b659b
出典データセット
uspto-grants-2011_01
特許番号
US07875615B2

関連ノート

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