Reaktion #41804

Reaktionsgleichung

1

2-Fluoro-3-(4-methyl-piperazin-1-yl)-6-nitro-phenylamine

hydroxylamine HCl

pyridine

→

2

3-Fluoro-4-(4-methyl-piperazin-1-yl)-benzene-1,2-diamine

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe resulting reaction mixture
2. 2
   EinengenThe crude product was concentrated
3. 3
   Sonstigeabsorbed onto silica gel
4. 4
   Sonstigepurified by flash chromatography (97:3 CH2Cl2/MeOH

Vorschrift

A 50 mL round bottom flask was charged with 1 (680 mg, 2.5 mmol), hydroxylamine HCl (191 mg, 2.75 mmol), pyridine (0.25 mL, 3.0 mmol) and ethanol (10 mL). The resulting reaction mixture was stirred at rt overnight. The crude product was concentrated, absorbed onto silica gel, and purified by flash chromatography (97:3 CH2Cl2/MeOH to give 2 as an orange solid. LCMS m/z 289.2 (MH+), tR=2.06 min.

Quelle