Phenyl 3-amino-2-(benzyloxy)-5-fluoro-6-methylbenzoate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of compound 65 (700 g, 1.84 mol) in THF (7 L) was cooled to 12° C. and stirred while adding a solution of Na2S2O4 (1599 g, 9.18 mol) in water (7.0 L) was added to the reaction with stirring. The exotherm was controlled by addition rate so that the reaction mixture temperature was below 17° C. The reaction mixture was then allowed to stir for 15 hours prior to adding 15.3 L EtOAc. The layers were separated and the organic layer was washed with successively with water (2×4 L and brine (1×4 L). The organic was dried over Na2SO4 and concentrated to give 699 g of a brownish solid that was recrystallized from heptane/toluene to afford 532 g (82.7%) of desired compound 66 obtained as an off-white solid. was added to the reaction with stirring The exotherm was controlled by addition rate so that the reaction mixture temperature was below 17° C to stir for 15 hours The layers were separated the organic layer was washed with successively with water (2×4 L and brine (1×4 L) The organic was dried over Na2SO4 concentrated