反应详情

A mixture of 18.0 g of 5-fluoro-2-nitrophenol, 29.0 g of caesium carbonate and 13.7 ml of 2-iodopropane in 119 ml of DMF is stirred at ambient temperature overnight. The mixture is concentrated under vacuum and the residue is taken up with 250 ml of water and extracted twice with 250 ml of ethyl acetate. The organic phases are washed twice with 200 ml of a saturated sodium chloride solution, dried over magnesium sulfate and concentrated under vacuum, so as to obtain 17 g of crude product. The crude product is purified on 400 g of silica, elution being carried out with cyclohexane/ethyl acetate (95/5), so as to obtain 13.0 g of 4-fluoro-1-nitro-2-(propan-2-yloxy)benzene in the form of a light yellow oil.

1. concentrationThe mixture is concentrated under vacuum
2. extractionextracted twice with 250 ml of ethyl acetate
3. washThe organic phases are washed twice with 200 ml of a saturated sodium chloride solution
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under vacuum
6. customso as to obtain 17 g of crude product
7. customThe crude product is purified on 400 g of silica, elution