HRID1510230

反应详情

EQUATION

反应方程式

HRID 1510230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customAfter removing the catalysts
  2. filtrationby filtration on celite pad
  3. customthe filtrate was evaporated in vacuo
  4. dissolutionThe residue was dissolved in 1N HCl (2 mL)
  5. washwashed with chloroform
  6. additionThe separated aqueous layer was adjusted to pH=7 by addition of saturated sodium bicarbonate solution
  7. extractionextracted with ethyl acetate
  8. washThe separated organic layer was washed with brine
  9. dry with materialdried over magnesium sulfate
  10. customevaporated in vacuo
  11. customThe residue was purified by column chromatography on silica gel