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

HRID 35467

반응식

HRID 35467 반응식
[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]

참가 물질

4

반응물 2

HCID 784Hydrogen Peroxide2회HCID 127592,3,5-Trimethylpyridine

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-edb4cdf3720449e2bd4e656c8d55258c
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766133

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