反应详情

温度

95 °C

To a flask equipped with an N2 inlet adaptor, add 2-(benzyloxy)-6-chloropyridine (1.63 g, 7.42 mmol), tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate (2.3 g, 7.42 mmol), tris(dibenzylideneacetone)dipalladium(0) (339.5 mg, 371.0 μmol), potassium phosphate (3.94 g, 18.55 mmol), tricyclohexylphosphine (208 mg, 0.742 mmol), water (4 mL) and 1,4-dioxane (40 mL). Flush with N2, then heat the mixture at 95° C. overnight under a nitrogen atmosphere. Filter and concentrate under vacuum to give a residue. Purify via silica gel flash column chromatography using a gradient of 0-30% ethyl acetate in petroleum ether to give the title compound as a white solid (2.6 g, 95.6%). MS (m/z): 367 (M+1).

1. customTo a flask equipped with an N2 inlet adaptor
2. customFlush with N2
3. filtrationFilter
4. concentrationconcentrate under vacuum
5. customto give a residue
6. customPurify via silica gel flash column chromatography