反应详情

A mixture of crude 1-[4-(4-fluoro-phenyl)-2-isopropyl-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl]-ethanone in 10% aq. HCl (800 mL) was heated at reflux for 2 h and then cooled to rt. The aqueous solution was washed with EtOAc (400 mL) and then was basified with NaOH pellets (˜120 g) to pH>12. The basic solution was extracted with CH2Cl2 (2×500 mL). The combined organic layers were washed with 1 N NaOH (400 mL), dried (MgSO4), and concentrated to give the crude product (100 g), which was used in the next reaction without further purification. HPLC: RT=6.89 min. MS (ESI): exact mass calcd. for C16H18FN3, 271.15; m/z found, 271.9 [M+H]+.

1. temperaturewas heated
2. temperatureat reflux for 2 h
3. washThe aqueous solution was washed with EtOAc (400 mL)
4. extractionThe basic solution was extracted with CH2Cl2 (2×500 mL)
5. washThe combined organic layers were washed with 1 N NaOH (400 mL)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated