反应详情

温度

5 °C

To a 3 L flask equipped with a mechanical stirrer was added 1-(4-chloro-3-methoxyphenyl)piperazine dihydrochloride (220 g, 0.73 mol, 1 equiv), CH2Cl2 (1000 mL), and water (1000 mL). The biphasic mixture was cooled to 5° C. with an ice-water bath. K2CO3 (506 g, 5 equiv) was added to the vigorously stirring solution in portions to minimize foaming. A solution of chloroacetyl chloride (124.4 g, 1.5 equiv) in CH2Cl2 (100 mL) was added dropwise from an addition funnel, while maintaining an internal temperature below 8° C. After 1 h, the cooling bath was removed, and the reaction warmed to room temperature. After an additional 1 h, the layers were partitioned. The aqueous phase was extracted with CH2Cl2 (2×300 mL), and the combined organic layers dried over 3:1 Na2SO4/K2CO3 (addition of K2CO3 helps the solution phase to become clear). After filtration, the filtrate was concentrated in vacuo, and the residue was dried for 16 h under vacuum to afford the product as an off-white solid (410 g, 92% yield).

1. customTo a 3 L flask equipped with a mechanical stirrer
2. temperaturewhile maintaining an internal temperature below 8° C
3. customthe cooling bath was removed
4. temperaturethe reaction warmed to room temperature
5. waitAfter an additional 1 h
6. customthe layers were partitioned
7. extractionThe aqueous phase was extracted with CH2Cl2 (2×300 mL)
8. dry with materialthe combined organic layers dried over 3:1 Na2SO4/K2CO3 (
9. additionaddition of K2CO3
10. filtrationAfter filtration
11. concentrationthe filtrate was concentrated in vacuo
12. customthe residue was dried for 16 h under vacuum