HRID1255834
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
A solution of methyl 3-{1-[(tert-butoxycarbonyl)amino]ethyl}benzoate (200 mg, 0.72 mmol) in 20% trifluoroacetic acid in dichloromethane (10 mL) was stirred at room temperature for 1.5 hours. After this time the mixture was concentrated under reduced pressure and the residue was dissolved in water and basified to pH 11 with aqueous ammonia. The mixture was extracted with ethyl acetate (2×15 mL) and the extracts were washed with brine (20 mL), dried (Na2SO4) and concentrated under reduced pressure to give methyl 3-(1-aminoethyl)benzoate (130 mg, 100%) as a pale yellow oil.
WORKUP
后处理
- concentrationAfter this time the mixture was concentrated under reduced pressure
- dissolutionthe residue was dissolved in water and basified to pH 11 with aqueous ammonia
- extractionThe mixture was extracted with ethyl acetate (2×15 mL)
- washthe extracts were washed with brine (20 mL)
- dry with materialdried (Na2SO4)
- concentrationconcentrated under reduced pressure