Hydrogen Peroxide → 2,3,5-Trimethyl-1-oxidopyridin-1-ium

HRID 35467

反応式

HRID 35467 の反応式
[OH:1]O.[N:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH3:10])[C:4]=1[CH3:11]>C(O)(=O)C>[CH3:11][C:4]1[C:5]([CH3:10])=[CH:6][C:7]([CH3:9])=[CH:8][N+:3]=1[O-:1]

参加物

4

反応物 2

HCID 784Hydrogen Peroxide2 回HCID 127592,3,5-Trimethylpyridine

生成物 1

HCID 104869072,3,5-Trimethyl-1-oxidopyridin-1-ium

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

420 ml of 30% hydrogen peroxide are added dropwise at room temperature to 246.4 g of 2,3,5-collidine and 2400 ml of glacial acetic acid. The solution is stirred at 80° overnight. The reaction mixture is then cooled to 40° , a further 420 ml of 30% hydrogen peroxide are added thereto and the mixture is heated to 80° for a further 24 hours. After evaporation in vacuo the residue is dissolved in 300 ml of water, whereupon the solution is made basic with conc. sodium hydroxide solution while cooling, saturated with sodium chloride and extracted three times with 1 1 of methylene chloride. The organic phases are dried over sodium sulphate and evaporated in vacuo. The residue is crystallized from ether/petroleum ether; there is obtained 2,3,5-trimethylpyridine 1-oxide of melting point 42°-44°.

後処理

  1. temperatureThe reaction mixture is then cooled to 40°
  2. temperaturethe mixture is heated to 80° for a further 24 hours
  3. customAfter evaporation in vacuo the residue
  4. dissolutionis dissolved in 300 ml of water, whereupon the solution
  5. temperaturewhile cooling, saturated with sodium chloride
  6. extractionextracted three times with 1 1 of methylene chloride
  7. dry with materialThe organic phases are dried over sodium sulphate
  8. customevaporated in vacuo
  9. customThe residue is crystallized from ether/petroleum ether

出典と根拠

ORDレコード
ord-edb4cdf3720449e2bd4e656c8d55258c
出典データセット
uspto-grants-1988_08
特許番号
US04766133

関連ノート

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