N-(3,5-Difluorophenyl)-4-nitrobenzenesulfonaMide, 97% synthesis

Yield:738-67-0 92%

Reaction Conditions:

with pyridine;dmap at 100; for 18 h;Concentration;

Steps:

A25 Preparation of intermediate 98:

A solution of 3,5-difluoroaniline (2 g; 15.49 mmol), 4-nitrobenzenesulfonyl chloride(3.61 g; 16.27 mmol) and 4-dimethylaminopyridine (37.9 mg; 0.31 mmol) in pyridine(60 mL) was heated at 100°C for 18h. After cooling down to rt, the solution wasevaporated under vacuum and taken-up in DCM. The organic layer was successivelywashed with iN aqueous solution of HC1 (x2), water and a saturated aqueous solution ofNaCl. Then, it was dried over MgSO4, filtered and evaporated under vacuum to give 4.5 g (92%, beige solid) of intermediate 98.

References:

WO2017/60406,2017,A1 Location in patent:Page/Page column 132