反应详情

A solution of 3-methoxy-4-[3-(2-methylphenyl)ureido]phenylacetic acid (0.7 g, Reference Example 31) in anhydrous dimethylformamide (25 ml) was treated sequentially with O-(7-azabenzotriazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate (0.85 g), diisopropylethylamine (0.54 g) and a solution of 3-(5-amino-pyrid-2-yl)propanoic acid ethyl ester [0.42 g, Reference Example 4(a)] in dimethylformamide (5 ml). After stirring at room temperature for 5 hours and standing over night the reaction mixture was evaporated. The residue was treated with ethyl acetate and the resulting solution was washed three times with water, then with brine and then evaporated. The residue was subjected to flash chromatography on silica gel eluting with a mixture of dichloromethane and methanol (97:3, v/v) to give the title compound (0.68 g) as a white foam.

1. waitstanding over night
2. customthe reaction mixture was evaporated
3. additionThe residue was treated with ethyl acetate
4. washthe resulting solution was washed three times with water
5. customwith brine and then evaporated
6. additionThe residue was subjected to flash chromatography on silica gel eluting with a mixture of dichloromethane and methanol (97:3