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

HRID 1733572

Reaktionsgleichung

Reaktionsgleichung von HRID 1733572
[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

Komponenten

3

Edukt 2

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

Produkt 1

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

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-664a29ce737d4a28899c2c1be96663e1
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04242515

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