反应详情

4-[(2,4-Dichloro-3-fluorophenyl)carbonyl]-2-piperazinone (I37)(0.25 g, 0.859 mmol) was dissolved in Dichloromethane (DCM) (2.147 ml) and triethyloxonium tetrafluoroborate (0.196 g, 1.031 mmol) was added. The solution was left to stir under an argon atmosphere for 18 hours. 6-(Methyloxy)-2-pyridinecarbohydrazide (I95) (0.172 g, 1.031 mmol) was added and the solution was left to stir under argon for a further 60 minutes. The Dichloromethane was removed under reduced pressure and 1-butanol (2.147 ml) was added and the reaction mixture was left at reflux for 3 hours. LCMS showed the product had formed so the solvent was removed under reduced pressure and the crude material was purified by flash chromatography (Biotage Isolera 4, 25 g cartridge) with a gradient of methanol 0-10% in Dichloromethane. The solvent was removed under reduced pressure to afford 0.285 g of material that was further purified using MDAP. The solvent was removed to afford the purified desired product in 0.108 g.

1. waitThe solution was left
2. waitthe solution was left
3. stirringto stir under argon for a further 60 minutes
4. customThe Dichloromethane was removed under reduced pressure and 1-butanol (2.147 ml)
5. additionwas added
6. waitthe reaction mixture was left
7. temperatureat reflux for 3 hours
8. customhad formed so the solvent
9. customwas removed under reduced pressure
10. customthe crude material was purified by flash chromatography (Biotage Isolera 4, 25 g cartridge) with a gradient of methanol 0-10% in Dichloromethane
11. customThe solvent was removed under reduced pressure