Phosphorus oxychloride → 2-Chloroisonicotinic acid

HRID 2738

反応式

HRID 2738 の反応式
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]

参加物

3

反応物 2

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

生成物 1

HCID 2369852-Chloroisonicotinic acid

反応条件

温度
120 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-8debf37587f1426b9a2fd8782e5c9316
出典データセット
uspto-grants-1998_03
特許番号
US05731310

関連ノート

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