HRID1799232

反应详情

EQUATION

反应方程式

HRID 1799232 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To an ethanol:THF (4:1, V/V, 7.5 mL) solution of 4-(2-cyclopropylethoxy)-N-((Z)-2-(4-cyclopropylphenyl)-1-{[(2-hydroxyethyl)amino]carbonyl}vinyl)benzamide (165 mg, 0.380 mmol) prepared in Example 1 (1d) was added tris(triphenylphosphine)rhodium(I) chloride (71 mg, 0.076 mmol). The mixture was stirred under a hydrogen atmosphere (rubber balloon) at 60° C. for 5 hours. The reaction solution was cooled to room temperature, and the solvent was evaporated. The residue was purified by alumina column chromatography (ethyl acetate to ethyl acetate:methanol, 10:1, V/V) to give 89 mg of the title compound (white powder, yield: 54%).

WORKUP

后处理

  1. temperatureThe reaction solution was cooled to room temperature
  2. customthe solvent was evaporated
  3. customThe residue was purified by alumina column chromatography (ethyl acetate to ethyl acetate:methanol, 10:1, V/V)