反应详情

O-(7-Azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphat (HATU; 1.23 g, 3.24 mmol, 3.00 eq) and N-methylmorpholine (0.71 ml, 0.66 g, 6.5 mmol, 6.0 eq) was added to a solution of 1-(2-methoxyethyl)-5-methyltriazole-4-carboxylic acid (200 mg, 1.08 mmol) and N-methylpyridazin-4-amine (118 mg, 1.08 mmol, 1.00 eq) in DMF (2.5 ml) and the mixture was stirred at room temperature for 4 d. After removal of the solvent, the residue was dissolved in dichloromethane, washed twice with sat. aq. NaHCO3 sol. and once with brine and dried over Na2SO4. Removal of the solvent under vacuum and chromatographic purification (CH:EtOAc) gave the title compound as a brown oil (200 mg, 64%, 95% purity).

1. customAfter removal of the solvent
2. dissolutionthe residue was dissolved in dichloromethane
3. washwashed twice with sat. aq. NaHCO3 sol. and once with brine
4. dry with materialdried over Na2SO4
5. customRemoval of the solvent
6. customunder vacuum and chromatographic purification (CH:EtOAc)