HRID705819

反应详情

EQUATION

反应方程式

HRID 705819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Pd/C (0.6 g, 10%, 50% water wet) was added to a solution of ethyl (2E)-3-(4-cyanophenyl)-2-propenoate (2.7 g, 13.42 mmol) in ethyl acetate (40 mL) under an argon atmosphere. It was mixed with TEA (3.74 mL, 26.8 mmol) and formic acid (2.57 mL, 67.1 mmol). The reaction mixture was refluxed at 90° C. under argon for 1 h. It was filtered through a Celite pad. The filtrate was then washed with water, 5% NaHCO3 solution and brine, dried over Na2SO4, and concentrated to provide the title compound as a pale yellow oil (2.65 g, 97% yield). LCMS: rt=2.94 min, [M+H+]=204.0

WORKUP

后处理

  1. filtrationIt was filtered through a Celite pad
  2. washThe filtrate was then washed with water, 5% NaHCO3 solution and brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated