反应详情

4-Aminophthalonitrile (3.60 g, 25.2 2.mmole) was dissolved in 8.6 mL of pyridine. Hexanoyl chloride (8.6 10, 61.5 mmole) was added and the mixture was stirred under N2 for 2 hours. The pyridine was distilled under vacuum until a yellow-orange residue was obtained. This residue was dissolved in dichloromethane and washed with 0.1 M HCl (5×15 mL) and then neutralized with aqueous sodium bicarbonate (3×50 mL). The organic solution was separated and dried over magnesium sulfate. Purification by column chromatography (silica, dichloromethane: methanol 5%) afforded 4.3 g (71% yield) of 4-hexanamidophthalonitrile as a light yellow compound.

1. distillationThe pyridine was distilled under vacuum until a yellow-orange residue
2. customwas obtained
3. washwashed with 0.1 M HCl (5×15 mL)
4. customThe organic solution was separated
5. dry with materialdried over magnesium sulfate
6. customPurification by column chromatography (silica, dichloromethane: methanol 5%)