HRID253721

反应详情

EQUATION

反应方程式

HRID 253721 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl acetoacetate (5.20 g), piridine-4-aldehyde (4.28 g), piperidine 0.4 ml) and AcOH (0.24 ml) are mixed in CH2Cl2 (150 ml) at room temperature under nitrogen atmosphere. The reaction mixture is stirred overnight and the solvent is removed. The residue is dissolved in EtOH (150 ml). 10% Pd/C (1.0 g) is added and reaction mixture is stirred at room temperature under hydrogen for 7 hours. Concentration under reduced pressure after Celite® filtration afford Ethyl 2-(4-pyridylmethyl)acetoacetate (8.0 g) as colorless oil.

WORKUP

后处理

  1. customthe solvent is removed
  2. dissolutionThe residue is dissolved in EtOH (150 ml)
  3. addition10% Pd/C (1.0 g) is added
  4. customreaction mixture
  5. stirringis stirred at room temperature under hydrogen for 7 hours
  6. concentrationConcentration under reduced pressure
  7. filtrationafter Celite® filtration