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With N-ethyl-N,N-diisopropylamine; In dimethyl sulfoxide; at 120℃; for 168h;
Heat a mixture of l,4-dichloro-2,3-dimethylpyridazine (6.06 g, 34.2 mmol), (S)-2- methyl-piperazine-1-carboxylic acid tert-butyl ester (6.88 g, 34.4 mmol) and dsopropylethylamine (30 ml, 172 mmol) in DMSO (30 mL) at 120 0C for 5 d. Cool and treat the mixture with additional (5)-2-methyl-piperazine-l-carboxylic acid tert-butyi ester (3.74 g, 18.7 mmol), and resume heating at 120 0C for an additional 2 d. Dilute the reaction mixture with EtOAc and wash with H2O and brine. Dry over Na2SO4, filter, and concentrate under reduced pressure. Purify the residue by flash silica gel chromatography (gradient of 20 to 50percent EtOAc in hexanes) to afford the title compound as a pale yellow foam (7.36 g, 63percent). ES/MS m/z (35Cl) 341.0 (M+l).
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