Reaktion #48587

Reaktionsgleichung

2,6-difluorobenzoic acid

4-amino-1H-pyrazole-3-carboxylic acid ethyl ester

EDC

HOBt

→

4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid ethyl ester

Lösungsmittel

DMF

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONadded
2. 2
   Sonstigethe solid formed
3. 3
   Filtrationcollected by filtration
4. 4
   Sonstigeair-dried

Vorschrift

A mixture of 2,6-difluorobenzoic acid (6.32 g, 40.0 mmol), 4-amino-1H-pyrazole-3-carboxylic acid ethyl ester (5.96 g, 38.4 mmol), EDC (8.83 g, 46.1 mmol) and HOBt (6.23 g, 46.1 mmol) in DMF (100 ml) was stirred at ambient temperature for 6 h. The mixture was reduced in vacuo, water added and the solid formed collected by filtration and air-dried to give 4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid ethyl ester as the major component of a mixture (15.3 g). (LC/MS: Rt 3.11, [M+H]+ 295.99).

Quelle