Reaktion #224
ord-9145f2f3fc8144728bdd2b390e48a7d0
Reaktionsgleichung
Lösungsmittel
Reaktionsbedingungen
Vorschrift
tert-butyl methylcarbamate (467 mg, 3.56 mmol) dissolved in dioxane (5ml) was added in one portion to 6-(2-morpholino-4-oxo-4H-pyrido[1,2-a]pyrimidin-9-yl)dibenzo[b,d]thiophen-2-yl trifluoromethanesulfonate (1000 mg, 1.78 mmol), TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (40.8 mg, 0.04 mmol) and (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (51.5 mg, 0.09 mmol) and cesium carbonate (2321 mg, 7.12 mmol) in dioxane (18mL) at 110 °C. The reaction flask was evacuated and blanketed with nitrogen 4X. The resulting suspension was stirred at 110 °C for 3 __ hours _. _ The crude product was purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 7M NH3/MeOH/DCM (50/50) and pure fractions were evaporated to dryness to afford tert-butyl methyl(6-(2-morpholino-4-oxo-4H-pyrido[1,2-a]pyrimidin-9-yl)dibenzo[b,d]thiophen-2-yl)carbamate (771 mg, 80 %) as a yellow solid. Used crude in the next reaction see EN01985-94