反应详情

A solution of 2,4,6-trichlorobenzenesulfonic acid chloride (3.00 g, 11 mmol) in 1,4-dioxane (50 ml) was added dropwise to a solution of 5-aminovaleric acid hydrochloride (1.50 g, 10 mmol) in 1 N sodium hydroxide solution (30 ml). The reaction mixture was stirred for 18 h at room temperature, and 1,4-dioxane was then distilled off in vacuo. The aqueous phase was extracted with ethyl acetate (3×50 ml) and then adjusted to pH 1 with concentrated hydrochloric acid. The acidic aqueous phase was extracted with ethyl acetate (3×60 ml). The combined organic phases were dried over sodium sulfate and concentrated in vacuo.

1. distillation1,4-dioxane was then distilled off in vacuo
2. extractionThe aqueous phase was extracted with ethyl acetate (3×50 ml)
3. extractionThe acidic aqueous phase was extracted with ethyl acetate (3×60 ml)
4. dry with materialThe combined organic phases were dried over sodium sulfate
5. concentrationconcentrated in vacuo