Methanol → 2-[2-(4-Bromo-phenoxy)-acetylamino]-isonicotinamide

To solution of (4-bromo-phenoxy)-acetic acid (100 mg, 0.43 mmol), 2-amino isonicotinamide (89.39 mg, 0.65 mmol) and DMAP (106 mg, 0.86 mmol) in DMF 5 ml was added PyBOP (452 mg, 0.86 mmol), and stirred room temperature. Reaction mixture was poured onto ice cold water, diluted by methanol/MC mixture (10%). The organic phase was separated, sequentially washed with aqueous sodium bicarbonate, brine and water, dried over anhydrous MgSO4, and concentrated. The residue was purified by PLC (EtoAC:Hexane:MeOH=3:6:1˜2:4:1) to afford 2-[2-(4-bromo-phenoxy)-acetylamino]-isonicotinamide as a colorless solid (0.083 g, 55% yield).

1. customReaction mixture
2. additionwas poured onto ice cold water
3. customThe organic phase was separated
4. washsequentially washed with aqueous sodium bicarbonate, brine and water
5. dry with materialdried over anhydrous MgSO4
6. concentrationconcentrated
7. customThe residue was purified by PLC (EtoAC:Hexane:MeOH=3:6:1˜2:4:1)

ORD-Eintrag

ord-c3dbf0970dbc4ba285fd1a4292ccaf6a

Quelldatensatz

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08394799B2