反应详情

To a solution of 3-(5-(4-chlorobenzyl)-6-isopropoxy-1-methyl-2,4-dioxo-1,2-dihydropyrido[2,3-d]pyrimidin-3(4H)-yl)propyl formate (55 mg, 0.13 mmol) in THF (6 mL) and water (6 mL) was added LiOH.H2O (10.9 mg, 0.26 mmol). The reaction was stirred at RT for 15 min then diluted with water (20 mL) and extracted with EA (3×15 mL). The combined organic layers were dried over Na2SO4 and concentrated to a residue which was purified by Prep HPLC to give 5-(4-chlorobenzyl)-3-(3-hydroxypropyl)-6-isopropoxy-1-methylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione (20 mg, 37% yield) as a white solid. 1H NMR (CDCl3) δ: 8.33 (s, 1H), 7.18 (s, 4H), 4.73 (s, 2H),), 4.68-4.68 (m, 1H), 4.28-4.15 (m, 2H), 3.69 (s, 3H), 3.52 (dd, J=11.8, 6.2 Hz, 2H), 3.16 (t, J=7.0 Hz, 1H), 1.97-1.82 (m, 2H), 1.34 (d, J=6.0 Hz, 6H). LCMS: MH+ 418 and TR=2.915 min.

1. extractionextracted with EA (3×15 mL)
2. dry with materialThe combined organic layers were dried over Na2SO4
3. concentrationconcentrated to a residue which
4. customwas purified by Prep HPLC