Water → HCID 86625714, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 5.0 g of 2,3-dimethoxy phenol in 1,3-dimethyl-2-imidazolidinone (65 ml) was added 7.28 g of potassium tert-butoxide, and was added dropwise a solution of 41.5 g of dibromo difluoromethane in 1,3-dimethyl-2-imidazolidinone (20 ml) over 30 minutes. The solution was stirred at 55° C. for 3 hours, and then water was added and the resulting mixture was extracted with Et2O. The organic layer was sequentially washed with 1 mol/L hydrochloric acid, water, and saturated brine, dried over MgSO4, then, the drying agent was separated by filtration and the solvent was evaporated under reduced pressure. The obtained residue was purified by column chromatography (silicagel 60; mobile phase: EtOAc/n-hexane=1/9 to 1/4; v/v) to obtain 2.21 g of the title compound (colorless oil).

Provenance & Evidence