反应 #1530380
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07511035B2
反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a sealed tube 1,1-dimethylethyl [2-(3-oxo-1-piperazinyl)ethyl]carbamate (1.7 g, 7.02 mmol), 6-(methyloxy)-1,5-naphthyridin-4-yl trifluoromethanesulfonate (2.17 g, 7.02 mmol), Pd2dba3 (436 mg, 0.421 mmol), rac-Binap (262 mg, 0.421 mmol), Cs2CO3 (4.81 g, 14.75 mmol) and 18-C-6 (186 mg, 0.702 mmol) in dioxane (35 mL) were combined and flushed with N2. After 15 min, the tube was sealed and heated to 100° C. while stirring rapidly. After 12 h, the solution was filtered, concentrated and the residue purified via column chromatography (silica, 1% MeOH in DCM (1% NH4OH)) yielding the title compound (1.5 g, 53%) as a burgundy foam: LCMS (ES) m/e 402 (M+H)+. flushed with N2 the tube was sealed After 12 h the solution was filtered concentrated the residue purified via column chromatography (silica, 1% MeOH in DCM (1% NH4OH))
来源 ID: ord-ac53345574d043ea8fa3e9e6e7420625