Reaktion #1865115

Reaktionsgleichung

6-amino-4-fluoronicotinonitrile

intermediate 21

6-amino-4-fluoronicotinonitrile

2-methoxyethylamine

DIPEA

→

title compound

6-amino-4-((2-methoxyethyl)amino)nicotinonitrile

Lösungsmittel

DMA

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was cooled to room temperature
2. 2
   Einengenconcentrated
3. 3
   SonstigeThe crude material was purified by normal phase chromatography (24 g silica gel cartridge, heptanes/EtOAc 100:0 to 0:100)
4. 4
   workup.ADDITIONThe product containing fractions
5. 5
   Einengenwere concentrated
6. 6
   Sonstigedried under vacuum

Vorschrift

A solution of 6-amino-4-fluoronicotinonitrile (intermediate 21, 1.10 g, 8.02 mmol) in DMA (20 ml) was treated with 2-methoxyethylamine (2.07 ml, 24.1 mmol) and DIPEA (4.20 mL, 24.1 mmol), heated to 50° C. and stirred for 15 h. The reaction mixture was cooled to room temperature and concentrated. The crude material was purified by normal phase chromatography (24 g silica gel cartridge, heptanes/EtOAc 100:0 to 0:100). The product containing fractions were concentrated and dried under vacuum to give the title compound as an off-white solid.

Quelle