HRID1391777

反应详情

EQUATION

反应方程式

HRID 1391777 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a flask containing 10% Pd/C catalyst under nitrogen was added ethyl (2E)-3-{2-methyl-4-[(phenylmethyl)oxy]phenyl}-2-propenoate (1.22 g, 4.12 mmol) in EtOH (15 mL) washing in with more EtOH (2×4 mL). The reaction vessel was placed under an atmosphere of hydrogen and stirred rapidly at ambient temperature for 19 h. The mixture was then filtered through a pad of celite washing with EtOH and the filtrate reduced under vacuum. The residue was the purified by SPE (silica, 20 g cartridge) eluting with cyclohexane:EtOAc (gradient 10:1 to 2:1) to afford the title compound (548 mg).

WORKUP

后处理

  1. washwashing in with more EtOH (2×4 mL)
  2. filtrationThe mixture was then filtered through a pad of celite
  3. washwashing with EtOH
  4. custompurified by SPE (silica, 20 g cartridge)
  5. washeluting with cyclohexane