3-DIFLUOROMETHYLPHENOL synthesis

Yield:405196-14-7 57%

Reaction Conditions:

with (bis-(2-methoxyethyl)amino)sulfur trufluoride in ethanol;dichloromethane at 20; for 12 h;

Steps:

Preparation procedure for 3-difluoromethylphenoI.To a solution of 3-hydroxybenzaldehyde (l.Olg, 0.0083 mol) in methylene chloride (3.3 mL) was added a solution of bis(2-methoxyethyl)aminosulfur trifluoride (3.09 g, 0.0140 mol) in methylene chloride (3.3 mL) followed by ethanol (95.0 μL, 0.00163 mol). The reaction mixture was stirred at room temperature for 12 hours. The mixture was then quenched carefully adding saturated aqueous sodium bicarbonate solution. The organic layer separated, washed with brine, dried over MgS04, and evaporated to give yellow oil. This oil was purified by column chromatography (0% to 50% ethyl acetate/heptane) to give the title compound (649 nag, 57%) as colorless oil.

References:

WO2012/39972,2012,A1 Location in patent:Page/Page column 23