2,4-Dimethylpyridine → HCID 22748777, Verbindung

HRID 1390334

Reaktionsgleichung

Reaktionsgleichung von HRID 1390334
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)[C:9]2[CH:10]=[CH:11][C:12](=O)[NH:13][CH:14]=2)=[CH:4][CH:3]=1.N1C=CC(C)=CC=1C.P(Cl)(Cl)([Cl:33])=O.[OH-].[NH4+]>>[Cl:33][C:12]1[CH:11]=[CH:10][C:9]([CH:8]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)[C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)=[CH:14][N:13]=1

Komponenten

5

Edukt 4

HCID 79362,4-DimethylpyridineHCID 14923Ammonium HydroxideHCID 24813Phosphorus oxychlorideHCID 227487685-[Bis-(4-Chlorophenyl)-Methyl]-2-Pyridone

Produkt 1

HCID 22748777HCID 22748777, Verbindung

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

To a mixture of 35.2 g. (0.11 mole) of 5-[bis-(4-chlorophenyl)-methyl]-2-pyridone and 11.8 g. (0.11 mole) of 2,4-lutidine, add 50.6 g. (0.33 mole) of phosphorous oxychloride (dropwise) while heating the reaction mixture at 80°. Then, heat the reaction mixture at 120° C. for six hours. Pour the reaction mixture onto ice, basify with ammonium hydroxide, extract with benzene and remove both the benzene and residual 2,4-lutidine by distillation. Distill the residue at about 195°-210° C. (0.01 mm) to obtain thereby about 30 g. of the product of this step as a yellow viscous oil.

Aufarbeitung

  1. additionTo a mixture of 35.2 g
  2. additionPour the reaction mixture onto ice
  3. extractionextract with benzene
  4. customremove both the benzene and residual 2,4-lutidine
  5. distillationby distillation
  6. distillationDistill the residue at about 195°-210° C. (0.01 mm)
  7. customto obtain

Quellen und Nachweise

ORD-Eintrag
ord-811dd63dab5743bb80fa0d1a1b9160cf
Quelldatensatz
uspto-grants-1979_02
Patentnummer
US04138488

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