Hydrogen Peroxide → 2-Chloro-5-methylpyridin-1-ium-1-olate

HRID 271065

反応式

HRID 271065 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][N:3]=1.[OH:9]O>C(O)(=O)C.O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][N+:3]=1[O-:9]

参加物

5

反応物 2

HCID 784Hydrogen PeroxideHCID 5813932-Chloro-5-methyl-pyridine

生成物 1

HCID 134316232-Chloro-5-methylpyridin-1-ium-1-olate収率 82%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To a solution of 2-chloro-5-methylpyridine (10 mL) in 155 mL of glacial acetic acid was added 19 mL of 30% aqueous hydrogen peroxide. The mixture was stirred at 80° C. for 8 hours. The mixture was diluted with 100 mL of water and then concentrated in a vacuum. The residue was made strongly alkaline with anhydrous sodium carbonate and shaken with 200 mL of chloroform. The solids were removed via filtration, and the filtrate was dried over sodium sulfate, filtered and concentrated to give 10.8 g of the 2-chloro-5-methylpyridine-N-oxide (82%). Mass Spec. M+H=144.

後処理

  1. concentrationconcentrated in a vacuum
  2. stirringshaken with 200 mL of chloroform
  3. customThe solids were removed via filtration
  4. dry with materialthe filtrate was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-c8e8c040bbd246b7bf3eebdc08915175
出典データセット
uspto-grants-2008_11
特許番号
US07452880B2

関連ノート

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