反应详情

温度

25 °C

A 25-mL single-neck round-bottomed flask equipped with a magnetic stirrer was charged with DMF (8 mL), 129a (160 mg, 0.38 mmol), HATU (505 mg, 1.33 mmol), DMAP (46 mg, 0.38 mmol), and triethylamine (1.0 mL). The mixture was heated at 25° C. for 0.5 h. Then MeNH2.HCl (266 mg, 3.8 mmol) was added and resulting mixture was stirred at 25° C. for 2.5 h. After this time the reaction was cooled to room temperature. It was then filtered and the filtrate was evaporated under reduced pressure. The residue was purified by prep-TLC developing with 1:20 methanol/dichloromethane to afford 129b (116 mg, 70%) as a black solid. MS-ESI: [M+H]+ 434.0

1. customA 25-mL single-neck round-bottomed flask equipped with a magnetic stirrer
2. customresulting mixture
3. temperatureAfter this time the reaction was cooled to room temperature
4. filtrationIt was then filtered
5. customthe filtrate was evaporated under reduced pressure
6. customThe residue was purified