反应详情

To a stirred solution of 5-benzyloxy-6-hydroxy-2-(3-phenyl-pyridin-2-ylmethyl)-pyrimidine-4-carboxylic acid (2-hydroxyethyl)-isopropylamide (166) in tetrahydrofuran (20 mL) were added triphenyl phosphine (66 mg, 0.25 mL) and DTAD (58 mg, 0.25 mmol) at room temperature. A yellow clear solution was formed, which was sonicated for 20 min. It was stirred at room temperature for 24 h. Silica thin layer chromatography was performed (5% methanol in dichloromethane, Rf=0.2). The mixture was concentrated under reduced pressure to get a crude product, which was purified by a preparative thin layer chromatography plate (mobile phase 5% methanol in dichloromethane) to get pure 9-benzyloxy-2-isopropyl-6-(3-phenyl-pyridin-2-ylmethyl)-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (167) (17 mg, 35.23%) as a yellow sticky solid.

1. customA yellow clear solution was formed
2. customwhich was sonicated for 20 min
3. concentrationThe mixture was concentrated under reduced pressure
4. customto get a crude product, which
5. customwas purified by a preparative thin layer chromatography plate (mobile phase 5% methanol in dichloromethane)