反应详情

2-piperazinone (4.00 g, 40 mmol, commercially available e.g. from Sigma-Aldrich) was dissolved in Dichloromethane (DCM) (125 mL) and to this was added triethylamine (6.69 mL, 48.0 mmol). This solution was then cooled with ice water. 2-Chloro-4-fluorobenzoyl chloride (8.49 g, 44.0 mmol, commercially available e.g. from Maybridge, Alfa Aesar or ABCR) was then diluted down with Dichloromethane (DCM) (25 mL), before being added via a pressure-equalizing dropping funnel. The solution was allowed to stir at room temperature overnight, and was then washed with sodium bicarbonate (100 ml), the solid was removed, and the remaining solution was washed again with sodium bicarbonate (100 ml) and brine (100 ml), before being dried over magnesium sulphate. The solvent was then removed in vacuo to afford crude product which was triturated with hexane then stirred in ethyl acetate at 80° C., before being filtered and air-dried to give 4-[(2-chloro-4-fluorophenyl)carbonyl]-2-piperazinone (5.179 g).

1. additionbefore being added via
2. washwas then washed with sodium bicarbonate (100 ml)
3. customthe solid was removed
4. washthe remaining solution was washed again with sodium bicarbonate (100 ml) and brine (100 ml)
5. dry with materialbefore being dried over magnesium sulphate
6. customThe solvent was then removed in vacuo
7. customto afford crude product which
8. customwas triturated with hexane
9. stirringthen stirred in ethyl acetate at 80° C.
10. filtrationbefore being filtered
11. customair-dried