Реакция #623606

Уравнение реакции

4-bromo-1-(formyl-amino)-6-methyl-2-nitrobenzoic acid

hydrochloric acid

→

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

Выход 88.1%

Растворители

water

Условия реакции

Обработка

1. 1
   ТемператураThe reaction mixture was cooled to room temperature
2. 2
   workup.ADDITIONtreated ice cold water
3. 3
   Экстракцияextracted with ethyl acetate (3×50 ml)
4. 4
   СушкаThe combined organic layers were dried over sodium sulfate
5. 5
   Концентрированиеconcentrated

Методика

A mixture of 4-bromo-1-(formyl-amino)-6-methyl-2-nitrobenzoic acid (20 g) (prepared according to US 2004/0167194 A1), concentrated hydrochloric acid (50 ml), and water (150 ml) was heated at 50° C. for 16 h. The reaction mixture was cooled to room temperature, treated ice cold water, and extracted with ethyl acetate (3×50 ml). The combined organic layers were dried over sodium sulfate and concentrated to give 1-amino-4-bromo-6-methyl-2-nitrobenzoic acid (16 g). 1H-NMR (400 MHz, CDCl3): 13.53 (bs, 1H), 7.56 (s, 1H), 7.07 (bs, 2H), 2.20 (s, 3H). LCMS: m/z=272.89 (M−H).

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