N,N-Diethylaniline → 5-(5-bromo-4-chloro-pyrimidin-2-ylamino)-pyridine-2-sulfonic Acid Amide

HRID 1182060Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1182060
[Br:1][C:2]1[C:3](O)=[N:4][C:5]([NH:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([NH2:18])(=[O:17])=[O:16])=[N:13][CH:14]=2)=[N:6][CH:7]=1.C(N(CC)C1C=CC=CC=1)C.P(Cl)(Cl)([Cl:33])=O>>[Br:1][C:2]1[C:3]([Cl:33])=[N:4][C:5]([NH:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([NH2:18])(=[O:17])=[O:16])=[N:13][CH:14]=2)=[N:6][CH:7]=1

Komponenten

4

Edukt 3

HCID 7061N,N-DiethylanilineHCID 24813Phosphorus oxychlorideHCID 178514724HCID 178514724, Verbindung

Produkt 1

HCID 589818655-(5-bromo-4-chloro-pyrimidin-2-ylamino)-pyridine-2-sulfonic Acid Amide

Versuchsvorschrift

175 mg (0.5 mmol) of 5-(5-bromo-4-hydroxy-pyrimidin-2-ylamino)-pyridine-2-sulfonic acid amide is refluxed with 20 mg of N,N-diethylaniline in 2 ml of phosphorus oxychloride for 3 hours. Then, it is cooled, poured onto ice and stirred for 30 minutes. The precipitated crystals are suctioned off, washed with water and acetonitrile and dried at 50° C. in a vacuum. Yield: 155 mg (85% of theory) of 5-(5-bromo-4-chloro-pyrimidin-2-ylamino)-pyridine-2-sulfonic acid amide.

Aufarbeitung

  1. temperatureThen, it is cooled
  2. additionpoured onto ice
  3. washwashed with water and acetonitrile
  4. customdried at 50° C. in a vacuum

Quellen und Nachweise

ORD-Eintrag
ord-b3e8bdee8da446c7aa36fba07465e597
Quelldatensatz
uspto-grants-2007_10
Patentnummer
US07288547B2

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