反应详情

A solution of [2-(4-(2-(3-methoxy-4-(3-o-tolyl-ureido)-phenyl)-acetylamino)-phenyl)-indan-2-yl]-acetic acid ethyl ester (0.06 g, Reference Example 16) in ethanol (10 mL) was treated with aqueous sodium hydroxide (300 μL, 1N) and the mixture was heated at reflux temperature for 8 hours and then left at room temperature overnight and then evaporated. The residue was treated with water (20 mL) and the mixture was warmed to aid dissolution. This solution was acidified to pH 1 by addition of hydrochloric acid (1N) when a precipitate was formed. The mixture was kept at 0° C. for 30 minutes then extracted with ethyl acetate. The ethyl acetate extract was dried over magnesium sulfate and then evaporated. The residual white solid was subjected to chromatography [gradient HPLC using 50% acetonitrile and water, 1 mL/minute] to give the title compound (0.03 g) as a white solid.

1. temperaturethe mixture was heated
2. temperatureat reflux temperature for 8 hours
3. customevaporated
4. additionThe residue was treated with water (20 mL)
5. temperaturethe mixture was warmed
6. dissolutiondissolution
7. additionThis solution was acidified to pH 1 by addition of hydrochloric acid (1N) when a precipitate
8. customwas formed
9. waitThe mixture was kept at 0° C. for 30 minutes
10. extractionthen extracted with ethyl acetate
11. extractionThe ethyl acetate extract
12. dry with materialwas dried over magnesium sulfate
13. customevaporated