反应详情

温度

25 °C

A solution of 3-cyclopentyl-2-(1-oxo-1H-phthalazin-2-yl)-propionic acid methyl ester (1.76 g, 5.85 mmol) in methanol (3.9 mL, 1.5M) was treated with a 4N aqueous sodium hydroxide solution (1.61 mL, 6.44 mmol) and stirred at 25° C. for 4 h. At this time, the reaction was concentrated in vacuo. The residue was diluted with water (100 mL) and was acidified with a 2N aqueous hydrochloric acid solution and then extracted with a solution of 90/10 methylene chloride/methanol (3×100 mL). The combined organics were dried over sodium sulfate, filtered and concentrated in vacuo to afford 3-cyclopentyl-2-(1-oxo-1H-phthalazin-2-yl)-propionic acid (1.58 g, 94%) as a white solid; ES+-HRMS m/e calcd for C16H18N2O3 [M+H+] 287.1390, found 287.1390.

1. concentrationAt this time, the reaction was concentrated in vacuo
2. additionThe residue was diluted with water (100 mL)
3. extractionextracted with a solution of 90/10 methylene chloride/methanol (3×100 mL)
4. dry with materialThe combined organics were dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo