Phosphorus oxychloride → 2-Chloro-5-(4-chlorophenyl)pyridine

HRID 1707090

反応式

HRID 1707090 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11](=O)[NH:12][CH:13]=2)=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:11]1[CH:10]=[CH:9][C:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)=[CH:13][N:12]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 102623725-(4-Chlorophenyl)-2-hydroxypyridine

生成物 1

HCID 100365542-Chloro-5-(4-chlorophenyl)pyridine

実験手順

A mixture of 22.27 g. of 5-(4-chlorophenyl)-2(1H)-pyridinone and 100 ml. of phosphorus oxychloride is refluxed for 16 hours, chilled and poured onto cracked ice. The solid formed is collected by filtration and then is dissolved in chloroform. The chloroform solution is washed with water and with saturated sodium bicarbonate and then is dried over magnesium sulfate. The solvent is evaporated at reduced pressure to yield 21.1 g. of the product of the Example as a gray solid, m.p. 113°-115° C.

後処理

  1. additionA mixture of 22.27 g
  2. temperaturechilled
  3. additionpoured
  4. customThe solid formed
  5. filtrationis collected by filtration
  6. dissolutionis dissolved in chloroform
  7. washThe chloroform solution is washed with water and with saturated sodium bicarbonate
  8. dry with materialis dried over magnesium sulfate
  9. customThe solvent is evaporated at reduced pressure
  10. customto yield 21.1 g

出典と根拠

ORDレコード
ord-d5590c08e35e4b66980320bedf345839
出典データセット
uspto-grants-1980_06
特許番号
US04209626

関連ノート

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