Phosphorus oxychloride → 2-Chloroisonicotinic acid

HRID 2738

반응식

HRID 2738 반응식
P(Cl)(Cl)([Cl:3])=O.[C:6]([OH:15])(=[O:14])[C:7]1[CH:12]=[CH:11][N+:10]([O-])=[CH:9][CH:8]=1>>[Cl:3][C:9]1[CH:8]=[C:7]([CH:12]=[CH:11][N:10]=1)[C:6]([OH:15])=[O:14]

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 261304-Pyridinecarboxylic acid, 1-oxide

생성물 1

HCID 2369852-Chloroisonicotinic acid

반응 조건

온도
120 °C

실험 절차

Phosphorus oxychloride (220.7 g) was added to isonicotinic acid N-oxide (50.064 g), and the mixture was stirred on an oil bath at 120° C. for 7 hours. The reaction mixture was slowly poured into ice water with vigorously stirring to precipitate light yellow crystals. The mixture was adjusted to approximately pH 4 with 4N NaOH aqueous solution. The resulting crystals were filtered out, washed with water, and dried by vacuum heating (60° C.) to obtain the above-captioned compound ([9]-(92)-467) (37.845 g).

후처리

  1. stirringwith vigorously stirring
  2. customto precipitate light yellow crystals
  3. filtrationThe resulting crystals were filtered out
  4. washwashed with water
  5. customdried by vacuum
  6. temperatureheating (60° C.)
  7. customto obtain the above-captioned compound ([9]-(92)-467) (37.845 g)

출처 및 근거

ORD 기록
ord-8debf37587f1426b9a2fd8782e5c9316
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731310

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