반응 #217032

반응 방정식

sodium hydrogen carbonate

1-iodo-2-nitro-4-fluoro-6-bromobenzene

tin (II) chloride dihydrate

ethanol

→

title compound

수율 76.0%

2-Iodo-3-bromo-5-fluoroaniline

수율 76.0%

용매

ethyl acetate

반응 조건

후처리

1. 1
   온도at reflux for 24 hours
2. 2
   여과Filter
3. 3
   세척wash the filtrate with saturated sodium hydrogen carbonate (200 mL) and water (200 mL)
4. 4
   건조Dry (MgSO4)
5. 5
   기타evaporate the solvent in vacuo
6. 6
   기타purify by silica gel chromatography

실험 절차

Treat 1-iodo-2-nitro-4-fluoro-6-bromobenzene (5.0 g, 14.46 mmol) with tin (II) chloride dihydrate (12 g, 58 mmol) in refluxing ethanol (150 mL). Stir at reflux for 24 hours, pour into a mixture of ethyl acetate (200 mL) and saturated sodium hydrogen carbonate (500 mL). Filter and wash the filtrate with saturated sodium hydrogen carbonate (200 mL) and water (200 mL). Dry (MgSO4), evaporate the solvent in vacuo and purify by silica gel chromatography to give the title compound as an off-white solid (3.45 g, 76%).

출처