N-(3,4-DIFLUOROPHENYL)-2,2-DIMETHYLPROPIONAMIDE synthesis

Yield:205756-46-3 99%

Reaction Conditions:

with triethylamine at 0 - 20; for 1 h;

Steps:

2

To a OC solution of 5.250 g (40.663 mmol) 3,4-difluoroanailine in 75 ml dichloromethane was added 5.487 mL (44.729mmol) pivaloyl chloride and 6.8 mL (48.796mmol) triethylamine. After stirring 1 h from OC to room temperature, the reaction mixture was diluted with CH₂Cl₂, washed with water and brine. The organic layer was dried over NaSθ4, filtered and concentrated in vacuo. Afforded 8.660 g (99%) N-(3,4- difluorophenyl)-2,2-dimethylpropanamide. ¹H NMR (CDCI3, 400 MHz) δ 7.68 - 7.63 (m, IH, ArH); 7.09 - 7.06 (m, 2H, ArH); 1.31 (s, 9H, O=C(CH₃)₃). ES MS+1 = 214.1.

References:

WO2009/9015,2009,A1 Location in patent:Page/Page column 28-29