反应详情

温度

70 °C

To a N2 purged round bottom flask was added 2-bromo-5-nitrophenol (29.0 g, 133 mmol, 1.0 eq.) followed by 16.8 mL (133 mmol, 1.0 eq) of ethyl chlorodifluoroacetate and 18.8 g of K2CO3 (133 mmol, 1.0 eq.). Anhydrous DMF (300 mL) was added and the mixture was stirred at 70° C. for 5 h. The mixture was cooled to RT and the solvent was removed. The obtained crude mixture was dissolved in CH2Cl2 (500 mL) and washed with 1 N NaOH (aq.). The organic layer was dried (MgSO4), filtered and evaporated. The crude material was further purified by column chromatography (0-5% EtOAc in hexanes) providing pure 1-bromo-2-difluoromethoxy-4-nitro-benzene.

1. temperatureThe mixture was cooled to RT
2. customthe solvent was removed
3. customThe obtained crude mixture
4. washwashed with 1 N NaOH (aq.)
5. dry with materialThe organic layer was dried (MgSO4)
6. filtrationfiltered
7. customevaporated
8. customThe crude material was further purified by column chromatography (0-5% EtOAc in hexanes)