반응 #164946

반응 방정식

2-Fluoro-5-iodo-3-nitro-benzoic acid methyl ester

SnCl2

→

3-amino-2-fluoro-5-iodo-benzoic acid methyl ester

수율 62.0%

용매

EtOAc

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도to reflux for two hours
3. 3
   농축concentrated under reduced pressure
4. 4
   workup.DISSOLUTIONThe residue was dissolved in 20 mL saturated aqueous NaHCO3
5. 5
   추출the aqueous mixture was extracted with EtOAc
6. 6
   세척The combined organic layers were washed with and brine
7. 7
   건조dried over Na2SO4
8. 8
   여과filtered
9. 9
   농축concentrated under reduced pressure

실험 절차

2-Fluoro-5-iodo-3-nitro-benzoic acid methyl ester (1.0 g, 3.08 mmol) and SnCl2 (2.33 g, 12.3 mmol) were added to 20 mL EtOAc, and the mixture was heated to reflux for two hours. The reaction mixture was cooled to room temperature and concentrated under reduced pressure. The residue was dissolved in 20 mL saturated aqueous NaHCO3, and the aqueous mixture was extracted with EtOAc. The combined organic layers were washed with and brine, dried over Na2SO4, filtered, and concentrated under reduced pressure to give 560 mg (62%) of 3-amino-2-fluoro-5-iodo-benzoic acid methyl ester, MS (M+H)=296.

출처