反応 #41806

反応方程式

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

溶媒

ethanol

反応条件

後処理

1. 1
   その他The resulting reaction mixture
2. 2
   濃縮The crude product was concentrated
3. 3
   その他absorbed onto silica gel
4. 4
   その他purified by flash chromatography (97:3 CH2Cl2/MeOH)

実験手順

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.

出典