반응 #41806

반응 방정식

1

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

methoxylamine HCl

pyridine

→

2

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

용매

ethanol

반응 조건

후처리

1. 1
   기타The resulting reaction mixture
2. 2
   농축The crude product was concentrated
3. 3
   기타absorbed onto silica gel
4. 4
   기타purified by flash chromatography (97:3 CH2Cl2/MeOH)

실험 절차

A 25 mL round bottom flask was charged with a suspension of 1 (600 mg, 2.2 mmol), methoxylamine HCl (202 mg, 2.42 mmol), and pyridine (0.22 mL, 2.6 mmol) in ethanol (9 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 303.2 (MH+), tR=2.40 mm.

출처