反应详情

4-[(2,4-Dichloro-3-fluorophenyl)carbonyl]-2-piperazinone (I37)(0.250 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 at room temperature under argon for 18 hours. 4-Methyl-2-pyrimidine carboximidohydrazide (I99) (0.156 g, 1.031 mmol) was dissolved in 1-butanol (2.147 ml) and this was added to the reaction mixture and this was left to stir under argon for a further 60 minutes. The dichloromethane was removed under reduced pressure and the reaction mixture was left at reflux for 4 hours. The solvent was removed under reduced pressure to afford a crude product of 0.690 g. The crude material was purified by flash chromatography (Biotage Isolera 4, 50 g cartridge) with a gradient of methanol 0-10% in Dichloromethane. The solvent was removed under reduced pressure to afford 0.223 g of material which was further purified using MDAP. The solvent was removed under reduced pressure to afford 0.090 g of crude material that was dissolved in methanol and loaded onto a 5 g SCX column. The column was washed with methanol and the desired compound was eluted off using 2M ammonia in methanol. The solvent was removed under reduced pressure to afford the purified product in 0.075 g.

1. waitThe solution was left
2. additionthis was added to the reaction mixture
3. waitthis was left
4. stirringto stir under argon for a further 60 minutes
5. customThe dichloromethane was removed under reduced pressure
6. waitthe reaction mixture was left
7. temperatureat reflux for 4 hours
8. customThe solvent was removed under reduced pressure
9. customto afford a crude product of 0.690 g
10. customThe crude material was purified by flash chromatography (Biotage Isolera 4, 50 g cartridge) with a gradient of methanol 0-10% in Dichloromethane
11. customThe solvent was removed under reduced pressure