反应详情

An oven dried flask under N2 was charged with 4-(tert-butyl-dimethyl-silanyloxymethyl)-6-chloro-pyridin-2-ylamine (11-5, 0.488 g, 1.79 mmol), 2-chloro-5-cyanothiazole (1-2, 0.310 g, 2.15 mmol), cesium carbonate (0.816 g, 2.50 mmol), tris(dibenzylideneacetone)dipalladium (0) (0.033 g, 0.040 mmol) and Xantphos (0.062 g, 0.060 mmol). Anhydrous dioxane, 6 mL, was added and the reaction was heated to reflux. After 3 hours the reaction was cooled to room temperature and stirred overnight. The reaction was diluted with water and extracted 3× with DCM. The extracts were dried over Na2SO4, filtered and concentrated. The resulting solid was triturated with ether, and filtered to afford the product as a tan solid.

1. customAn oven dried flask under N2
2. temperaturethe reaction was heated to reflux
3. extractionextracted 3× with DCM
4. dry with materialThe extracts were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe resulting solid was triturated with ether
8. filtrationfiltered