反应详情

1,2,3,4-Tetrahydro-6-methyl-7-bromo pyrido[2,3-b]pyrazine (0.15 g, 1 mmol), 2-chloro 3,6-difluoro-benzyl bromide (0.16 g, 1.05 mmol), KI (0.016 mmol, 0.01 g) in acetonitrile was subjected to microwave irradiation at 130° C. for 20 min. The solvent was stripped off and the crude residue was re-dissolved in CH2Cl2, washed with aqueous NaHCO3 solution. Upon drying, the residue was chromatographed, eluting with a mixture of hexanes-EtOAc (7:3) to furnish pure desired product (0.086 g 23%). The undesired N-alkylation product was also obtained and the structural differentiation was based on NOE NMR experiment.

1. customirradiation at 130° C. for 20 min
2. washwashed with aqueous NaHCO3 solution
3. customUpon drying
4. customthe residue was chromatographed
5. washeluting with a mixture of hexanes-EtOAc (7:3)