反应详情

To solution of (2,4-dichloro-phenoxy)acetic acid (192.7 mg, 0.87 mmol), 5-amino nicotinic acid methyl ester (200 mg, 1.31 mmol) and DIPEA (169.8 mg, 1.31 mmol) in DMF 5 mL was added EDC (252 mg, 1.31 mmol) and HOBt (177.62 mg, 1.31 mmol) at room temperature. Reaction mixture was stirred at room temperature, poured onto ice cold water, extracted with ethyl acetate, sequentially washed with aqueous sodium bicarbonate, brine and water, dried over anhydrous MgSO4, and concentrated. The residue was purified by flash silica gel column chromatography (EtoAC:Hexane=1:9˜1:1) to give 3-[2-(2,4-dichloro-phenoxy)-acetylamino]-N-(3-morpholine-4-yl-propyl)-benzamide as a colorless solid (0.185 g, 60% yield).

1. customReaction mixture
2. additionpoured onto ice cold water
3. extractionextracted with ethyl acetate
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 flash silica gel column chromatography (EtoAC:Hexane=1:9˜1:1)