Реакция #623607

Уравнение реакции

1-amino-4-bromo-6-methyl-2-nitrobenzoic acid

→

1,2-diamino-6-methylbenzoic acid

Выход 69.0%

Растворители

methanol

Условия реакции

Обработка

1. 1
   Фильтрацияfiltered through Celite under nitrogen atmosphere
2. 2
   ДругоеEvaporation of methanol and purification by chromatography (hexane/ethyl acetate 40:60)

Методика

A suspension of 1-amino-4-bromo-6-methyl-2-nitrobenzoic acid (16 g) and Pd/C (3.2 g) in methanol (400 ml) was stirred under hydrogen (1 bar) for 48 h and filtered through Celite under nitrogen atmosphere. Evaporation of methanol and purification by chromatography (hexane/ethyl acetate 40:60) gave 1,2-diamino-6-methylbenzoic acid (6.7 g) as a brown solid (6.7 g). 1H-NMR (400 MHz, CDCl3): 12.09 (bs, 1H), 6.73 (d, 1H), 6.13 (d, 1H), 1.98 (s, 3H). LCMS: m/z=167.11 (M+H)

Источник