Reaktion #2260899

Reaktionsgleichung

3-amino-6-bromo-5-trifluoromethyl-pyrazine-2-carboxylic acid

Intermediate 2

3-amino-6-bromo-5-trifluoromethyl-pyrazine-2-carboxylic acid

5-amino-4-(pyridin-2-yl)-1H-pyrazole

HATU

N-methylmorpholine

→

title compound

3-Amino-6-bromo-N-(4-(pyridin-2-yl)-1H-pyrazol-5-yl)-5-(trifluoromethyl)pyrazine-2-carboxamide

Lösungsmittel

water

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationthe resulting yellow precipitate was filtered under vacuum
2. 2
   Waschenwashed with water (20 ml)
3. 3
   workup.ADDITIONMeOH (150 ml) was added to the solid
4. 4
   Sonstigethe suspension ultrasonicated
5. 5
   Sonstigeto give a fine suspension
6. 6
   FiltrationThe suspension was filtered under vacuum
7. 7
   Waschenthe solid was rinsed with MeOH (20 ml)
8. 8
   Sonstigedried under vacuum at 45° C. for 1.5 hours

Vorschrift

A mixture comprising 3-amino-6-bromo-5-trifluoromethyl-pyrazine-2-carboxylic acid (Intermediate 2) (0.179 g, 0.624 mmol), 5-amino-4-(pyridin-2-yl)-1H-pyrazole (0.1 g, 0.624 mmol), HATU (0.237 g, 0.624 mmol) and N-methylmorpholine (0.123 ml, 1.249 mmol) in DMF (5 ml) was stirred at 80° C. for 2.5 hours. After cooling to RT, the mixture was diluted with water (40 ml) and the resulting yellow precipitate was filtered under vacuum and washed with water (20 ml). MeOH (150 ml) was added to the solid and the suspension ultrasonicated to give a fine suspension. The suspension was filtered under vacuum and the solid was rinsed with MeOH (20 ml) and dried under vacuum at 45° C. for 1.5 hours to afford the title compound as a yellow solid.

Quelle