反应详情

2-piperazinone (0.350 g, 3.5 mmol, commercially available from e.g. Sigma-Aldrich) was dissolved in dichloromethane (DCM) (15 mL), and to this was added triethylamine (0.585 mL, 4.20 mmol). The solution was then cooled to 0° C. before 3-chloro-4-fluoro-2-methylbenzoyl chloride (I58) (0.797 g, 3.85 mmol) in Dichloromethane (DCM) (5 mL) was added dropwise. The solution was stirred, under argon, for 30 minutes before the solvent was evaporated in vacuo. The remaining residue was then re-dissolved in DCM (50 mL) and washed with water (20 mL), a saturated solution of sodium bicarbonate (20 mL) and brine (20 mL). The organic phase was then dried over anhydrous sodium sulphate, which was then filtered off and the solvent was evaporated in vacuo. The remaining solid was then stirred in hexane (30 mL) at 55° C. for 30 minutes, before being filtered to yield the product in 0.843 g.

1. additionwas added dropwise
2. customwas evaporated in vacuo
3. dissolutionThe remaining residue was then re-dissolved in DCM (50 mL)
4. washwashed with water (20 mL)
5. dry with materialThe organic phase was then dried over anhydrous sodium sulphate, which
6. filtrationwas then filtered off
7. customthe solvent was evaporated in vacuo
8. stirringThe remaining solid was then stirred in hexane (30 mL) at 55° C. for 30 minutes
9. filtrationbefore being filtered
10. customto yield the product in 0.843 g