反应 #41806

反应方程式

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

溶剂

ethanol

反应条件

后处理

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

实验过程

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.

来源