反应详情

A solution of 3-{(3,4-dimethoxy-benzyl)-[({[3-methoxy-4-(3-o-tolylureido)phenyl]-acetyl}-N-methylamino)-acetyl]-amino}-propionic acid ethyl ester [2.0 g, Reference Example 4(a)] in ethanol (50 ml) was treated with sodium hydroxide (3.5 ml, 1M). After stirring at room temperature for 3 hours the mixture was concentrated to dryness. The residue was dissolved in water (12 ml) and the pH of the solution was adjusted to 1.0 by addition of concentrated hydrochloric acid (0.25 ml) and then extracted three times with dicliloromethiane. The resultant solid was collected and recrystallised twice from 20% aqueous isopropanol to give 3-{(3,4-dimethoxy-benzyl)-[({[3-methoxy-4-(3-o-tolylureido)phenyl]-acetyl}-N-methylamino)-acetyl]-amino}-propionic acid (Compound C) as a white solid (0.25 g,), m.p. 183-187° C.

1. concentrationwas concentrated to dryness
2. dissolutionThe residue was dissolved in water (12 ml)
3. additionthe pH of the solution was adjusted to 1.0 by addition of concentrated hydrochloric acid (0.25 ml)
4. extractionextracted three times with dicliloromethiane
5. customThe resultant solid was collected
6. customrecrystallised twice from 20% aqueous isopropanol