反应详情

温度

80 °C

A mixture of 7-benzyl-5,6,7,8-tetrahydro-2-(methoxymethyl)pyrido[3,4-d]pyrimidin-4(3H)-one (2.01 g, 7.04 mmol), phosphorus oxychloride (5.16 mL, 56.35 mmol) and N,N-dimethylaniline (0.89 mL, 7.04 mmol) in 1,2-dichloroethane was heated to 80° C. for two h. The mixture was allowed to cool to r.t. and poured over crushed ice (100 mL). The mixture was made basic (pH=˜8) by the addition of saturated aqueous sodium bicarbonate and extracted with ethyl acetate (200 mL). The organic layer was dried over magnesium sulfate and concentrated to leave a dark oil which was purified by silica gel chromatography (ethyl acetate/hexane gradient) to yield 1.76 g (82%) of the title compound as a brown oil.

1. temperatureto cool to r.t.
2. additionpoured
3. extractionextracted with ethyl acetate (200 mL)
4. dry with materialThe organic layer was dried over magnesium sulfate
5. concentrationconcentrated
6. customto leave a dark oil which
7. customwas purified by silica gel chromatography (ethyl acetate/hexane gradient)