p-Toluenesulfonic acid → HCID 178428862, Verbindung

HRID 488726Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 488726
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=1[Cl:15].C([O:19][CH2:20][CH3:21])(=O)C.[C:22]1(C)C=CC(S(O)(=O)=O)=C[CH:23]=1>C1C=CC=CC=1>[CH3:22][C:23]1[CH:21]=[C:20]([OH:19])[C:7]2[C:2](=[C:3]([C:8]3[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=3[Cl:15])[CH:4]=[N:5][CH:6]=2)[N:1]=1

Komponenten

5

Edukt 3

HCID 6101p-Toluenesulfonic acidHCID 8857Ethyl AcetateHCID 222673263-(2,4-Dichlorophenyl)pyridin-4-amine

Produkt 1

HCID 178428862HCID 178428862, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

A solution of B1 (2.41 g, 10.1 mmole), ethyl acetate (1.31 g, 10.1 mmole) and p-toluenesulfonic acid (70 mg) in benzene (50 ml) is heated at reflux for 2 h. during which 10 ml of solvent is removed by distillation. After evaporation, the residue is added to boiling diphenyl ether (10 ml) and heating is continued for 1 h; then the solution is cooled and poured into high boiling petroleum ether with vigorous stirring. The resulting solid formed is filtered off and washed with diethyl ether to give the product B2.

Aufarbeitung

  1. customis removed by distillation
  2. customAfter evaporation
  3. additionthe residue is added
  4. temperatureheating
  5. temperaturethen the solution is cooled
  6. additionpoured
  7. customThe resulting solid formed
  8. filtrationis filtered off
  9. washwashed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-f82d02bce378407597b41adcb05d8c71
Quelldatensatz
uspto-grants-2005_12
Patentnummer
US06974808B2

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