Reaktion #163124

Reaktionsgleichung

2,5,6-trichloronicotinonitrile

DIEA

5-cyclopropyl-1H-pyrazol-3-amine

→

title compound

Ausbeute 43.9%

2,5-Dichloro-6-(5-cyclopropyl-1H-pyrazol-3-ylamino)nicotinonitrile

Ausbeute 43.9%

Lösungsmittel

n-BuOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas cooled to room temperature
2. 2
   Einengenconcentrated
3. 3
   workup.ADDITIONThe resulting residue was diluted with 10 ml ACN
4. 4
   SonstigeThe solids that formed
5. 5
   Filtrationwere then filtered
6. 6
   Waschenwashed with cold ACN
7. 7
   Sonstigedried
8. 8
   Sonstigecollected

Vorschrift

To a solution of 2,5,6-trichloronicotinonitrile (Method 44, 1.0 g, 4.8 mmol) and DIEA (0.81 g, 6.2 mmol) in n-BuOH (5 ml) was added 5-cyclopropyl-1H-pyrazol-3-amine (2.3 g, 19.3 mmol). The reaction was heated to 60° C. for 2 hours, at which point the reaction was cooled to room temperature and concentrated. The resulting residue was diluted with 10 ml ACN, and stored at 0° C. for 1 hour. The solids that formed were then filtered, washed with cold ACN, dried and collected to give the title compound (0.62 g, 43%). MS: Calcd.: 294. Found: [M+H]+ 295.

Quelle