Reaktion #1179425

Reaktionsgleichung

ammonium chloride

(R)-2-(4-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-nitropyridin-2-ylamino)-2-(4-fluorophenyl)ethanol

ammonium acetate

→

(R)-2-(5-Amino-4-(5-cyclopropyl-1H-pyrazol-3-ylamino)pyridin-2-ylamino)-2-(4-fluorophenyl)ethanol

Lösungsmittel

MeOH THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe resulting mixture was stirred for another 30 minutes
2. 2
   SonstigeThe Zn dust was removed by filtration
3. 3
   Waschenwashed with EtOAc (20 ml)
4. 4
   SonstigeThe organic layer was separated
5. 5
   Waschenwashed with brine (10 ml)
6. 6
   Trocknendried over sodium sulfate
7. 7
   Einengenconcentrated
8. 8
   SonstigeThe crude product was used directly for the next step without further purification

Vorschrift

To a suspension of (R)-2-(4-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-nitropyridin-2-ylamino)-2-(4-fluorophenyl)ethanol (Method 94, 0.14 g, 0.36 mmol) and zinc dust (0.12 g, 1.78 mmol) in MeOH-THF (1:1, 16 ml) was slowly added saturated ammonium chloride (2.0 ml). The reaction mixture was stirred at 25° C. for 1 hour, to which was then added saturated ammonium acetate solution (5 ml). The resulting mixture was stirred for another 30 minutes. The Zn dust was removed by filtration and washed with EtOAc (20 ml). The organic layer was separated, washed with brine (10 ml), dried over sodium sulfate, and concentrated. The crude product was used directly for the next step without further purification. MS: Calcd.: 368; Found: [M+H]+ 369.

Quelle