Reaktion #1274860

Reaktionsgleichung

(S)-4,6-dichloro-N-[1-(4-fluorophenyl)ethyl]pyrimidine-2-amine

2-aminopyrazine

tripotassium phosphate

→

objective compound

Ausbeute 58.2%

(S)-6-Chloro-N2-[1-(4-fluorophenyl)ethyl]-N4-(pyrazin-2-yl)pyrimidine-2,4-diamine

Ausbeute 58.2%

Lösungsmittel

1,4-dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto degassing
2. 2
   workup.ADDITIONThe reaction solution was diluted with ethyl acetate
3. 3
   WaschenThe solution was washed in turn with water and brine
4. 4
   Trocknendried over magnesium sulfate
5. 5
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
6. 6
   Sonstigethe obtained residue was purified by silica gel column chromatography

Vorschrift

To 1.37 g of (S)-4,6-dichloro-N-[1-(4-fluorophenyl)ethyl]pyrimidine-2-amine (Reference Example 1), 460 mg of 2-aminopyrazine, 277 mg of 4,5-bis(diphenylphosphino)-9,9′-dimethylxanthene, 2.04 g of tripotassium phosphate and 248 mg of tris(dibenzylideneacetone)(chloroform)dipalladium, was added 30 ml of 1,4-dioxane, and the mixture was subjected to degassing and was substituted with argon gas, and then was stirred at 100° C. for 2 hours. The reaction solution was diluted with ethyl acetate. The solution was washed in turn with water and brine and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure, and then the obtained residue was purified by silica gel column chromatography to obtain 960 mg of the objective compound as pale yellow powder.

Quelle