反应详情

In a large microwave vial, 2-chloro-5-nitropyridine (386 mg, 2.436 mmol) was dissolved in 4 ml of dimethylformamide. 3,3-dimethyl-2,3-dihydro-1-benzofuran-4-ol (Intermediate 57, 400 mg) and potassium carbonate (2.02 g, 14.62 mmol) were added. The reaction mixture was heated under microwave irradiation during 30 minutes at 110 C (Biotage Initiator). The reaction mixture was filtered. The filtrated solid was washed with dichloromethane (30 ml). The volatiles were evaporated under vacuum. The residue was purified by silica gel chromatography (Companion instrument, 120 g cartridge) with cyclohexane as eluent to afford the title compound (470 mg).

1. temperatureThe reaction mixture was heated under microwave irradiation during 30 minutes at 110 C (Biotage Initiator)
2. filtrationThe reaction mixture was filtered
3. washThe filtrated solid was washed with dichloromethane (30 ml)
4. customThe volatiles were evaporated under vacuum
5. customThe residue was purified by silica gel chromatography (Companion instrument, 120 g cartridge) with cyclohexane as eluent