Phosphorus oxychloride → 2-Chloroisonicotinic acid

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

반응물 2

HCID 24813Phosphorus oxychloride

HCID 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

stirringwith vigorously stirring
customto precipitate light yellow crystals
filtrationThe resulting crystals were filtered out
washwashed with water
customdried by vacuum
temperatureheating (60° C.)
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
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05731310

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