反应详情

2-(4,5-Dibromo-6-oxopyridazin-1(6H)-yl)-N-(pyridin-4-ylmethyl)acetamide (50 mg, 124 μmol) in dioxane-water (1:1, 2 mL) was stirred with triethylamine (52 μL, 372 μmol) and 2,5,5-trimethylhexan-2-amine (16 mg, 112 μmol) at 90° C. for 26 hours. After completion of the reaction, the solvent was removed by vacuum distillation, and the residue was mixed with saturated aqueous sodium chloride and extracted with chloroform three times. The combined organic layer was dried over anhydrous magnesium sulfate, and the solvent was removed by vacuum distillation. The resulting residue was purified by silica gel chromatography (chloroform/methanol=10/1) to give the desired product (13 mg, 25% yield).

1. customAfter completion of the reaction
2. customthe solvent was removed by vacuum distillation
3. additionthe residue was mixed with saturated aqueous sodium chloride
4. extractionextracted with chloroform three times
5. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
6. customthe solvent was removed by vacuum distillation
7. customThe resulting residue was purified by silica gel chromatography (chloroform/methanol=10/1)