反应详情

Tris(dibenzylideneacetone)dipalladium (840 mg) and 4,5-bis(diphenyl-phosphino)-9,9-dimethylxanthene (1.6 g) and sodium tert-butoxide (6.6 g) were added to a solution of morpholine (2 ml) and 2-bromo-5-iodo-pyridine (7.8 g) in toluene (230 ml), and the mixture was stirred under nitrogen atmosphere at room temperature overnight. Water and ethyl acetate were added to the mixture and the organic layer was separated, washed with a saturated brine, dried over magnesium sulfate and concentrated in vacuo. The resulting residue was purified by column chromatography (silica gel; hexane:ethyl acetate=9:1→7:3) to give the titled compound (5.07 g). MS (m/z): 243/245 [M+H]+.

1. customthe organic layer was separated
2. washwashed with a saturated brine
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe resulting residue was purified by column chromatography (silica gel; hexane:ethyl acetate=9:1→7:3)