反应详情

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

1. temperatureat reflux for 24 hours
2. filtrationFilter
3. washwash the filtrate with saturated sodium hydrogen carbonate (200mL) and water (200mL)
4. dry with materialDry (MgSO4)
5. customevaporate the solvent in vacuo
6. custompurify by silica gel chromatography