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

HRID 230137

반응식

HRID 230137 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 134316232-Chloro-5-methylpyridin-1-ium-1-olate수율 82%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-383281804cd8434b8d76fb1f59486e8b
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566708B2

연결된 노트

불러오는 중…