反应详情

Add a solution of LiOH.H2O (2.87 g, 68.4 mmol) in water (60 mL) to a rapidly stirred solution of 5-[5-(2-hydroxy-phenyl)-isoxazol-3-yl]-pentanoic acid ethyl ester (3.96 g, 13.7 mmol) in dioxane (120 mL) and stir at room temperature overnight. After 1 hour, acidify to pH 1 with 5N HCl solution and concentrate to remove the majority of the dioxane. Add water to residue and place in refrigerator overnight. Filter out solids, wash with water, dry in a 50° C. vacuum oven for 6 hours to afford the title compound (3.11 g, 87%). MS (IS) 262 (M+1)+.

1. waitAfter 1 hour
2. concentrationconcentrate
3. customto remove the majority of the dioxane
4. customplace in refrigerator overnight
5. filtrationFilter out solids
6. washwash with water
7. customdry in a 50° C. vacuum oven for 6 hours