反应详情

To solution of 2-[2-(2,4-dichloro-phenoxy)-acetylamino]-isonicotinic acid (80.0 mg, 0.24 mmol), 2-piperidine-1-yl-ethylamine (46.2 mg, 0.05 ml, 0.36 mmol), EDC (69.0 mg, 0.36 mmol) and HOBt (48.7 mg, 0.36 mmol) in DMF 4 ml was added DIPEA (46.5 mg, 0.06 ml, 0.36 mmol), and stirred. Reaction mixture was then partitioned between ethyl acetate and 10% HCl. The organic phase was washed with brine, dried over anhydrous MgSO4, and concentrated. The residue was purified by preparative-TLC (n-Hexane:EtoAC:MeOH=6:3:1) to afford 2-[2-(2,4-dichloro-phenoxy)-acetylamino]-N-(2-piperidine-1-yl-ethyl)-isonicotinamide as a yellow solid (14.3 mg, 13.3% yield).

1. customReaction mixture
2. customwas then partitioned between ethyl acetate and 10% HCl
3. washThe organic phase was washed with brine
4. dry with materialdried over anhydrous MgSO4
5. concentrationconcentrated
6. customThe residue was purified by preparative-TLC (n-Hexane:EtoAC:MeOH=6:3:1)