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 ethyl (2E)-2-cyano-3-phenylacrylate (1.2 g) in ethanol (30 mL) was added 10% Palladium hydroxide (0.3 g) and the mixture was hydrogenated at 3 atms. for 2 hours. After removing the catalysts by filtration on celite pad, the filtrate was evaporated in vacuo. The residue was dissolved in 1N HCl (2 mL) and washed with chloroform. The separated aqueous layer was adjusted to pH=7 by addition of saturated sodium bicarbonate solution and extracted with ethyl acetate. The separated organic layer was washed with brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel to afford ethyl 3-amino-2-benzylpropanoate (388 mg).
WORKUP
后处理
- customAfter removing the catalysts
- filtrationby filtration on celite pad
- customthe filtrate was evaporated in vacuo
- dissolutionThe residue was dissolved in 1N HCl (2 mL)
- washwashed with chloroform
- additionThe separated aqueous layer was adjusted to pH=7 by addition of saturated sodium bicarbonate solution
- extractionextracted with ethyl acetate
- washThe separated organic layer was washed with brine
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customThe residue was purified by column chromatography on silica gel