تفاعل #89545

معادلة التفاعل

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

SnCl2

NaHCO3

→

title compound

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

المذيبات

EtOAc

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling at rt
2. 2
   استخلاصThe mixture was extracted with EtOAc
3. 3
   غسيلthe organic layer was washed with brine
4. 4
   ترشيحfiltered through diatomaceous earth
5. 5
   تجفيفdried over Na2SO4

الإجراء التجريبي

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]+.

المصدر