Reaktion #48579

Reaktionsgleichung

4-Nitropyrazole-3-carboxylic acid

4-amino-1-Boc-piperidine

EDC

HOAt

→

4-[(4-nitro-1H-pyrazole-3-carbonyl)-amino]-piperidine-1-carboxylic acid tert-butyl ester

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent was removed by evaporation under reduced pressure
2. 2
   Sonstigethe residue triturated with water (250 ml)
3. 3
   FiltrationThe resultant cream solid was collected by filtration
4. 4
   Waschenwashed with water
5. 5
   Sonstigethen dried under vacuum

Vorschrift

4-Nitropyrazole-3-carboxylic acid (7.3 g; 15.9 mmol) was added to a stirred solution of 4-amino-1-Boc-piperidine (10.2 mg; 51 mmol), EDC (10.7 g; 55.8 mmol), and HOAt (55.8 g; 19.1 mmol) in DMF (100 ml), and then stirred at room temperature overnight. The solvent was removed by evaporation under reduced pressure and the residue triturated with water (250 ml). The resultant cream solid was collected by filtration, washed with water then dried under vacuum to give 13.05 g of 4-[(4-nitro-1H-pyrazole-3-carbonyl)-amino]-piperidine-1-carboxylic acid tert-butyl ester (LC/MS: Rt 2.50, [M+H]+ 340).

Quelle