Hydrogen Peroxide → 2-Chloro-4-methylpyridine 1-oxide

HRID 1039081ノート

反応式

HRID 1039081 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N:3]=1.OO.C([O-])([O-])=[O:12].[Na+].[Na+]>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N+:3]=1[O-:12]

参加物

5

反応物 3

HCID 784Hydrogen PeroxideHCID 10340Sodium CarbonateHCID 772482-Chloro-4-methylpyridine

生成物 1

HCID 124874842-Chloro-4-methylpyridine 1-oxide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
65 °C

実験手順

2-chloro-4-methylpyridine (10 g, 80 mmol) was dissolved in acetic acid (100 ml). Hydrogen peroxide (31%, 86.8 g, 80.7 ml, 790 mmol)) was added in 4 portions and the solution stirred under nitrogen at 65° C. for 18 hours. The mixture was poured into ice water (300 ml), and solid Na2CO3 added until the solution was alkaline. The mixture was extracted with DCM (3×300 ml), the organic fractions combined, washed with sodium thiosulfate (1M, 100 ml), brine, dried over Na2SO4, and the volatiles removed in vacuum to give the titled compound.

後処理

  1. additionadded until the solution
  2. extractionThe mixture was extracted with DCM (3×300 ml)
  3. washwashed with sodium thiosulfate (1M, 100 ml), brine
  4. dry with materialdried over Na2SO4
  5. customthe volatiles removed in vacuum

出典と根拠

ORDレコード
ord-6a615a75ed284508a0b89c6529a24c42
出典データセット
uspto-grants-2013_10
特許番号
US08552022B2

反応ノート

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