反应详情

温度

60 °C

To a stirred solution of N-(3-aminopropyl)-7-[3-fluoro-4-({[(2-fluoro-5-methylphenyl)amino]carbonyl}amino)phenoxy]thieno[3,2-b]pyridine-2-carboxamide (125 mg, 0.24 mmol) and N,N-diisopropylethylamine (77 mg, 0.60 mmol) in 10 ml of anhydrous DMF was added methyl bromoacetate (92 mg, 0.60 mmol). The mixture was heated at 60° C. for 1 hour and poured into 100 ml of water with vigorous stirring. The precipitates were filtered and dried in vacuo to give the crude, which was purified by silica gel chromatography eluting with 3˜4% of MeOH in CHCl3 to afford dimethyl 2,2′-({3-[({7-[3-fluoro-4-({[(2-fluoro-5-methylphenyl)amino]carbonyl}amino)phenoxy]thieno[3,2-b]pyridin-2-yl}carbonyl)amino]propyl}imino)diacetate as white solid. Yield: 140 mg, 88%.

1. filtrationThe precipitates were filtered
2. customdried in vacuo
3. customto give the crude, which
4. customwas purified by silica gel chromatography
5. washeluting with 3˜4% of MeOH in CHCl3