反应详情

温度

150 °C

A mixture of N-(4-tert-butylphenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine (0.066 g, 0.23 mmol), 2-chloro-3-(methylsulfonyl)pyridine (Ponticello et al, J. Org. Chem., 44(17), 1979), (0.088 g, 0.47 mmol) and N,N-diisopropylethlamine (0.041 mL, 0.23 mmol) was heated in a sealed tube via microwave (Emrys Optimizer model, Personal Chemistry) for 30 min at 150° C. The reaction mixture was cooled to r.t. and poured into water (20 mL). The mixture was extracted with ethyl acetate (2×20 mL). The combined organic layers were washed with brine, dried over magnesium sulfate and concentrated to leave an oil which was purified by silica gel chromatography (ethyl acetate/hexane gradient) to give the title compound as a white solid (0.049 g).

1. temperatureThe reaction mixture was cooled to r.t.
2. extractionThe mixture was extracted with ethyl acetate (2×20 mL)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated
6. customto leave an oil which
7. customwas purified by silica gel chromatography (ethyl acetate/hexane gradient)