反应详情

温度

160 °C

Homophthalic anhydride (1.5 g, 9.25 mmol), 3-buten-1-amine (1.129 ml, 11.10 mmol), and 4 A molecular sieves (300 mg) were combined in toluene (15 ml) and heated to 160° C. in a microwave for 40 minutes. The reaction mixture was diluted with CH2Cl2 and the slurry was filtered over CELITE. The filtrate was concentrated in vacuo and the resulting residue was purified by column chromatography (gradient elution, 10-20% EtOAc/Hexane) to afford the title compound (0.75 g, 36%) as an oil. LCMS (ES+) m/z 216.03 (M+H)+.

1. filtrationthe slurry was filtered over CELITE
2. concentrationThe filtrate was concentrated in vacuo
3. customthe resulting residue was purified by column chromatography (gradient elution, 10-20% EtOAc/Hexane)