Reaktion #172102

Reaktionsgleichung

2,6-dichloro-3-cyano-5-fluoropyridine

1-aminocyclopentanecarboxamide hydrochloride

DIEA

Water

→

1-(6-chloro-5-cyano-3-fluoropyridin-2-ylamino)cyclopentanecarboxamide

Ausbeute 49.0%

Lösungsmittel

DMSO

EtOAc

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organic phase was separated
2. 2
   Trocknendried over Na2SO4
3. 3
   Einengenconcentrated in vacuo
4. 4
   SonstigeThe residue was purified by a silica gel column
5. 5
   Wascheneluted with 50-100% EtOAc in hexane

Vorschrift

A solution of 2,6-dichloro-3-cyano-5-fluoropyridine (250 mg, 1.30 mmol), 1-aminocyclopentanecarboxamide hydrochloride (214 mg, 1.30 mmol) and DIEA (0.650 mL, 3.73 mmol) in DMSO (3 mL) was stirred at 95 C for 4 h. Water and EtOAc were added. The organic phase was separated, dried over Na2SO4, concentrated in vacuo. The residue was purified by a silica gel column, eluted with 50-100% EtOAc in hexane to give 1-(6-chloro-5-cyano-3-fluoropyridin-2-ylamino)cyclopentanecarboxamide (180 mg).

Quelle