Sodium Azide → 5-bromo-2-(1H-pyrazol-1-yl)pyrimidine-4,6-diamine

HRID 2401168

Reaktionsgleichung

Reaktionsgleichung von HRID 2401168
[Br:1][C:2]1[C:3]([NH2:14])=[N:4][C:5]([N:9]2[CH:13]=[CH:12][CH:11]=[N:10]2)=[N:6][C:7]=1Cl.[N-:15]=[N+]=[N-].[Na+]>O1CCOCC1>[Br:1][C:2]1[C:3]([NH2:14])=[N:4][C:5]([N:9]2[CH:13]=[CH:12][CH:11]=[N:10]2)=[N:6][C:7]=1[NH2:15]

Komponenten

4

Edukt 2

HCID 33557Sodium AzideHCID 866770175-bromo-6-chloro-2-(1H-pyrazol-1-yl)pyrimidin-4-amine2×

Produkt 1

HCID 534678255-bromo-2-(1H-pyrazol-1-yl)pyrimidine-4,6-diamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of 0.10 g (0.37 mmol) of 5-bromo-6-chloro-2-(1H-pyrazol-1-yl)pyrimidine-4-amine (Intermediate 5) and 0.05 g (0.77 mmol) of sodium azide in dioxane (10 mL) was stirred at 80° C. for 6 h. The solvent was then evaporated, and the residue dissolved in methanol, Pd on charcoal added (10 mg) and hydrogenated for 30 min. The solvent was again evaporated and the residue crystallizes from ethanol.

Aufarbeitung

  1. customThe solvent was then evaporated
  2. dissolutionthe residue dissolved in methanol
  3. additionPd on charcoal added (10 mg)
  4. customThe solvent was again evaporated
  5. customthe residue crystallizes from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-3c2b21ac9b854f46891fa63dd5814f14
Quelldatensatz
uspto-grants-2014_08
Patentnummer
US08796284B2

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