反应详情

2-piperazinone (1 g, 9.99 mmol, commercially available from e.g. Sigma-Aldrich) and triethylamine (2.78 mL, 19.98 mmol) were dissolved in Dichloromethane (DCM) (25 mL) at 0° C. 2,3-dichloro-4-methylbenzoyl chloride (I71) (2.232 g, 9.99 mmol) dissolved in Dichloromethane (DCM) (25 mL) was added dropwise and the solution stirred to room temperature overnight. Solvents were removed in vacuo and the residue was partitioned between ethyl acetate (50 mL) and saturated sodium bicarbonate solution (25 mL). The aqueous phase was extracted with ethyl acetate (3×50 mL). The combined organic extracts were washed with water (2×50 mL), brine (50 mL), dried over anhydrous sodium sulfate and concentrated to a crude solid. A 100 mg sample was purified by MDAP to afford product in 69 mg.

1. additionwas added dropwise
2. customSolvents were removed in vacuo
3. customthe residue was partitioned between ethyl acetate (50 mL) and saturated sodium bicarbonate solution (25 mL)
4. extractionThe aqueous phase was extracted with ethyl acetate (3×50 mL)
5. washThe combined organic extracts were washed with water (2×50 mL), brine (50 mL)
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated to a crude solid
8. customA 100 mg sample was purified by MDAP
9. customto afford product in 69 mg