反应详情

温度

70 °C

A mixture of 5A (40 mg, 0.123 mmol), 5-methylisoxazol-3-amine (30.1 mg, 0.307 mmol) and sodium t-butoxide (29.5 mg, 0.307 mmol) in THF (1.5 mL) was heated at 70° C. for 2 h, the cooled to room temperature. The solvent was removed and the residue was purified by ISCO column chromatography (4 g column, MeOH/DCM=0-10%) to give 51A (23 mg, 48%). HPLC Rt=3.043 min (Chromolith SpeedROD 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA, 4 min gradient, monitored at 220 nm), [M+H]=388.

1. temperaturethe cooled to room temperature
2. customThe solvent was removed
3. customthe residue was purified by ISCO column chromatography (4 g column, MeOH/DCM=0-10%)