Phosphorus oxychloride → 2-Chloro-5-(phenylthio)pyridine

HRID 372734

反応式

HRID 372734 の反応式
[C:1]1([S:7][C:8]2[CH:9]=[CH:10][C:11](=O)[NH:12][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:17])=O.P(Cl)(Cl)(Cl)(Cl)Cl>>[Cl:17][C:11]1[CH:10]=[CH:9][C:8]([S:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:13][N:12]=1

参加物

4

反応物 3

HCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 203265625-(Phenylthio)-2-pyridone

生成物 1

HCID 111953972-Chloro-5-(phenylthio)pyridine

実験手順

A suspension of 5-(phenylthio)-2-pyridone (4.06 g., .02 mole) in 50 ml. of phosphorous oxychloride containing 10 g. of phosphorous pentachloride is heated at reflux for 6 hours. Excess phosphorous oxychloride is removed in vacuo and the residue is poured onto icewater mixture. The mixture is cooled and the pH adjusted to neutral with dilute aqueous sodium hydroxide. The resultant suspension is extracted with methylene chloride. The combined extracts are washed with water, dried and evaporated in vacuo to yield 2-chloro-5-(phenylthio)pyridine.

後処理

  1. temperatureat reflux for 6 hours
  2. customExcess phosphorous oxychloride is removed in vacuo
  3. additionthe residue is poured onto icewater mixture
  4. temperatureThe mixture is cooled
  5. extractionThe resultant suspension is extracted with methylene chloride
  6. washThe combined extracts are washed with water
  7. customdried
  8. customevaporated in vacuo

出典と根拠

ORDレコード
ord-423277c83c734a099258532c889e5f3e
出典データセット
uspto-grants-1978_05
特許番号
US04092321

関連ノート

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