Acetyl bromide → 4-Bromo-6,6'-dimethyl-2,2'-bipyridine

HRID 1586927ノート

反応式

HRID 1586927 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([N+]([O-])=O)[CH:5]=[C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[N:10]=2)[N+:7]=1[O-].[OH-].[Na+].C([Br:24])(=O)C>P(Br)(Br)Br>[Br:24][C:4]1[CH:3]=[C:2]([CH3:1])[N:7]=[C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[N:10]=2)[CH:5]=1

参加物

5

反応物 3

HCID 10482Acetyl bromideHCID 14798Sodium HydroxideHCID 110321326,6'-Dimethyl-4-nitro-2,2'-bipyridine-N-oxide

生成物 1

HCID 118322434-Bromo-6,6'-dimethyl-2,2'-bipyridine

試薬・触媒・溶媒 1

HCID 24614Phosphorus tribromide溶媒

実験手順

6,6'-Dimethyl-4-nitro-2,2'-bipyridine-N-oxide (0.50 g, 2.0 mmoles) was dissolved in acetyl bromide (10.0 ml) and phosphorus tribromide (2.5 ml). After refluxing for 1.5 hours the mixture was poured into 100 g ice and the solution was neutralized with 30% sodium hydroxide solution. The mixture was extracted with chloroform, the chloroform phase was dried and evaporated. The product was purified by means of flash chromatography.

後処理

  1. temperatureAfter refluxing for 1.5 hours the mixture
  2. extractionThe mixture was extracted with chloroform
  3. dry with materialthe chloroform phase was dried
  4. customevaporated
  5. customThe product was purified by means of flash chromatography

出典と根拠

ORDレコード
ord-1c109e159f09407a99c521bc04376b94
出典データセット
uspto-grants-1993_06
特許番号
US05216134

反応ノート

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