Реакция #41806

Уравнение реакции

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

Растворители

ethanol

Условия реакции

Обработка

1. 1
   ДругоеThe resulting reaction mixture
2. 2
   КонцентрированиеThe crude product was concentrated
3. 3
   Другоеabsorbed onto silica gel
4. 4
   Другоеpurified by flash chromatography (97:3 CH2Cl2/MeOH)

Методика

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.

Источник