Br[C:2]1[C:3]([N+:8]([O-:10])=[O:9])=[N:4][CH:5]=[CH:6][N:7]=1.C([O-])([O-])=O.[K+].[K+].[CH3:17][N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1>O1CCOCC1>[CH3:17][N:18]1[CH2:23][CH2:22][N:21]([C:6]2[CH:5]=[N:4][C:3]([N+:8]([O-:10])=[O:9])=[CH:2][N:7]=2)[CH2:20][CH2:19]1In a 15 mL argon dried microwave reaction vial, was added bromonitropyrazine (300 mg, 1.47 mmoL, Eq: 1.00) and K2CO3 (264 mg, 1.91 mmoL, Eq: 1.3) under argon to give a light yellow slurry. N-methylpiperazine (192 mg, 212 μl, 1.91 mmol, Eq: 1.3) was added dropwise and the reaction mixture became an orange yellow thick slurry. Heated to 70° C. in an oil bath for 1.5 hrs then stirred at room temperature overnight. The reaction mixture was diluted with dioxane (10 mL), filtered through a fitted funnel and washed with DCM (10 mL). The combined filtrate and washes were concentrated to dryness to give a yellow solid (328 mg, yield 89%) which was used directly in the next step.
Wird geladen…
