HRID1054364
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
N-(4-Bromo-phenyl)-2-chloro-acetamide (0.3 g, 1.21 mmol) was dissolved in anhydrous toluene (10 ml). Pyrrolidine (0.3 ml, 3.63 mmol) was added dropwise to the mixture, which was then heated to reflux and stirred overnight. The toluene was removed under reduced pressure and the residue was dissolved in ethyl acetate. Saturated ammonium chloride was added and the aqueous layer was extracted twice with ethyl acetate. The organics were combined, washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. Yield 0.22 g, 65%. LCMS method: 2, RT: 2.62 min; MI: 283-285 [M+1].
WORKUP
后处理
- temperaturewas then heated
- temperatureto reflux
- customThe toluene was removed under reduced pressure
- dissolutionthe residue was dissolved in ethyl acetate
- additionSaturated ammonium chloride was added
- extractionthe aqueous layer was extracted twice with ethyl acetate
- washwashed with brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo