HRID1747820
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
To a solution of tert-butyl 3-hydroxyazetidine-1-carboxylate (1 g), triethylamine (1.2 mL) and DMAP (7 mg) in THF (10 ml) was added benzoylchloride (0.81 g) under ice-cooling. The reaction mixture was stirred at room temperature for 2 hr, water was added, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was dissolved in ethyl acetate (10 mL), and 4M hydrogen chloride in ethyl acetate solution (3 mL) was added. The reaction mixture was stirred at room temperature for 2 hr, and the precipitate was collected by filtration to give the title compound (710 mg).
WORKUP
后处理
- temperaturecooling
- extractionthe mixture was extracted with ethyl acetate
- dry with materialThe extract was dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in ethyl acetate (10 mL)
- addition4M hydrogen chloride in ethyl acetate solution (3 mL) was added
- stirringThe reaction mixture was stirred at room temperature for 2 hr
- filtrationthe precipitate was collected by filtration