反应详情

To a stirred mixture of 4-amino-3-chlorobenzoic acid (58.3 mmol, 10 g), tert-butyl piperazine-1-carboxylate (58.3 mmol, 10.86 g) and triethylamine (146 mmol, 20.31 mL, 14.74 g) in dichloromethane (200 mL) was added N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (69.9 mmol, 13.41 g). The reaction was stirred for 24 hours then was diluted with ethyl acetate and water. The organic layer was separated, dried (magnesium sulfate) and concentrated under reduced pressure. Diethyl ether was added and the solid was filtered off to give the title compound (15.4 g).

1. customThe organic layer was separated
2. dry with materialdried (magnesium sulfate)
3. concentrationconcentrated under reduced pressure
4. additionDiethyl ether was added
5. filtrationthe solid was filtered off