Dichloromethane → HCID 57732141, compound

Participants

Reaction Steps

TFA (750 L, 9.7 mmol) was added to a solution of 6-{[(2,4-dimethoxybenzyl)(1,3-thiazol-2-yl)amino]sulfonyl}-N-[4-(trifluoromethyl)benzyl]nicotinamide (Preparation 88, 1.15 g, 1.94 mmol) in methylene chloride (12 mL, 180 mmol). After 30 min, the reaction mixture was diluted with ether. Triethylamine was added until basic to neutralize the residual TFA. Celite was added, and the mixture was concentrated in vacuo. The residue was purified on the Isco (120 g SiO2 cartridge, chloroform to 12% MeOH in chloroform). The appropriate fractions were concentrated in vacuo. The residue was treated with acetonitrile, generating a white precipitate. The volume was reduced in vacuo, and the solids were collected via filtration, washing with acetonitrile. The off-white product was dried under vacuum (428 mg, 47%).

Provenance & Evidence