反应详情

温度

65 °C

To a solution of 5.0 g (25.2 mmol) of 5-ethylamino-3-methylsulfanyl-1,2,4-triazine-6-carbaldehyde in 125 mL of THF was added 6.7 g (37.8 mmol) of 3,5-dimethoxyphenylacetonitrile followed by 17.4 g (126.1 mmol) of potassium carbonate. The reaction mixture was warmed at 65° C. for 2 days, concentrated under vacuum, diluted with ethyl acetate, and washed three times with a saturated solution of sodium bicarbonate, once with water and brine. The organic phase was dried over magnesium sulfate, filtered, decolorized with charcoal, filtered through celite, and concentrated to give a dark orange oil. The crude oil was chromatographed through silica eluted with 2:2:6 to 2:3:5 dichloromethane/ethyl acetate/hexane to give 5.4 g (59%) of the title compound as a yellow amorphous solid. MS (APCI) (m+1)/z 358.1.

1. concentrationconcentrated under vacuum
2. additiondiluted with ethyl acetate
3. washwashed three times with a saturated solution of sodium bicarbonate
4. dry with materialThe organic phase was dried over magnesium sulfate
5. filtrationfiltered
6. filtrationfiltered through celite
7. concentrationconcentrated
8. customto give a dark orange oil
9. customThe crude oil was chromatographed through silica
10. washeluted with 2:2:6 to 2:3:5 dichloromethane/ethyl acetate/hexane