反应详情

温度

160 °C

To a solution of 1,7-dichloroisoquinoline-3-carbonitrile (500 mg, 2.24 mmol) in NMP (5 mL) was added (S)-tert-butyl 3-aminopyrrolidine-1-carboxylate (460 mg, 2.46 mmol) and Et3N (453 mg, 4.48 mmol). The solution was heated to 160° C. for 30 minutes in a microwave reactor. The reaction was quenched with H2O (20 mL) and extracted with EtOAc (3×10 mL). The organic layers were combined and concentrated in vacuo. The crude product was purified by column chromatography eluting with ethyl acetate and petroleum ether (EtOAc/PE=1:10 to 1:5 gradient) to give the title compound (660 mg, 79%). ESI-MS m/z [M+H-tert-butyl]+ 317.

1. customThe reaction was quenched with H2O (20 mL)
2. extractionextracted with EtOAc (3×10 mL)
3. concentrationconcentrated in vacuo
4. customThe crude product was purified by column chromatography
5. washeluting with ethyl acetate and petroleum ether (EtOAc/PE=1:10 to 1:5 gradient)