反应详情

温度

70 °C

A solution of ethyl 7-(2-phenyl-3-p-tolyl-7,8-dihydropyrido[2,3-b]pyrazin-5(6H)-yl)heptanoate (1.07 g, 2.338 mmol) in THF (12 ml) and water (6 ml) was treated with LiOH (0.560 g, 23.38 mmol) and stirred at 70° C. for 18 hours. After cooling to RT, the reaction mixture was concentrated in vacuo. The residue was diluted with water (20 ml) and the pH was adjusted to pH˜4 using 2M HCl. The aqueous portion was extracted with EtOAc (2×20 ml). The organic extracts were washed with brine, dried (MgSO4) and evaporated under vacuum. The residue was dissolved in hot (˜80° C.) ethanol (20 ml) and water (˜15 ml) was added until the solution became turbid. Upon cooling a solid precipitated. The mixture was kept cold for 72 hours.

1. temperatureAfter cooling to RT
2. concentrationthe reaction mixture was concentrated in vacuo
3. additionThe residue was diluted with water (20 ml)
4. extractionThe aqueous portion was extracted with EtOAc (2×20 ml)
5. washThe organic extracts were washed with brine
6. dry with materialdried (MgSO4)
7. customevaporated under vacuum
8. dissolutionThe residue was dissolved in hot (˜80° C.) ethanol (20 ml) and water (˜15 ml)
9. additionwas added until the solution
10. temperatureUpon cooling a solid
11. customprecipitated
12. waitThe mixture was kept cold for 72 hours