反应详情

温度

160 °C

A mixture of 4-chloro-7-(5-(trifluoromethyl)pyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine (0.035 g, 0.00011 mol), 3-methoxyaniline (0.018 mL, 0.00016 mol) in acetonitrile (0.5 mL, 0.01 mol) and 47% HI (0.05 mL, 0.0007 mol) was heated at 160° C. for 20 minutes in in a sealed tube via microwave. After cooling to r.t., the mixture was poured into saturated aqueous sodium bicarbonate (5 mL) and extracted with ethyl acetate (10 mL). The organic layer was washed with brine and dried over magnesium sulfate. Concentrated to leave a brown solid. Residue was purified by flash chromatography over silica gel (ethyl acetate/hexane gradient 0 to 100%) to give 0.196 g of a white foam.

1. temperatureAfter cooling to r.t.
2. extractionextracted with ethyl acetate (10 mL)
3. washThe organic layer was washed with brine
4. dry with materialdried over magnesium sulfate
5. concentrationConcentrated
6. customto leave a brown solid
7. customResidue was purified by flash chromatography over silica gel (ethyl acetate/hexane gradient 0 to 100%)