Reaktion #1179407

Reaktionsgleichung

NH4Cl

(S)-ethyl 6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-2-[1-(4-fluorophenyl)ethylamino]-5-nitropyrimidine-4-carboxylate

(S)-Ethyl 6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-2-[1-(4-fluorophenyl)ethylamino]-5-nitropyrimidine-4-carboxylate

→

title compound

Ausbeute 94.0%

(S)-Ethyl 5-amino-6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-2-[1-(4-fluorophenyl)ethylamino]pyrimidine-4-carboxylate

Ausbeute 94.0%

Lösungsmittel

EtOH THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationfiltered through a plug of celite with EtOAc (100 ml)
2. 2
   ExtraktionThe resulting aqueous layer was extracted with EtOAc (2×100 ml)
3. 3
   Sonstigedried
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated

Vorschrift

To a suspension of (S)-ethyl 6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-2-[1-(4-fluorophenyl)ethylamino]-5-nitropyrimidine-4-carboxylate (Method 10; 0.7 g, 1.5 mmol) and zinc dust (0.5 g, 7.7 mmol) in EtOH:THF (1:1, 20 ml) was slowly added saturated aqueous NH4Cl solution (3 ml). After 1 hour, the reaction mixture was cooled to 0° C., to which was added saturated NH4OAc solution (10 ml). The resulting mixture was allowed to stir for 10 minutes at 0° C. and then filtered through a plug of celite with EtOAc (100 ml). The resulting aqueous layer was extracted with EtOAc (2×100 ml), dried, filtered, and concentrated to give the title compound (0.60 g, 92%) which was used without further purification.

Quelle