Реакция #89545

Уравнение реакции

5-fluoro-3-methyl-2-nitrobenzoic acid

SnCl2

NaHCO3

→

title compound

2-Amino-5-fluoro-3-methylbenzoic acid

Растворители

EtOAc

Условия реакции

Обработка

1. 1
   ТемператураAfter cooling at rt
2. 2
   ЭкстракцияThe mixture was extracted with EtOAc
3. 3
   Промывкаthe organic layer was washed with brine
4. 4
   Фильтрацияfiltered through diatomaceous earth
5. 5
   Сушкаdried over Na2SO4

Методика

A mixture of 5-fluoro-3-methyl-2-nitrobenzoic acid (4.86 g, 24.42 mmol) and SnCl2 (16.5 g, 72.36 mmol) in EtOAc was heated at 70° C. overnight. After cooling at rt, the pH was adjusted to 7-8 with satd. aq. NaHCO3. The mixture was extracted with EtOAc, and the organic layer was washed with brine, filtered through diatomaceous earth, and dried over Na2SO4 to provide the title compound, which was used without further purification. ESI-MS (m/z): 170 [M+1]+.

Источник