HRID2267482

反应详情

EQUATION

反应方程式

HRID 2267482 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To the solution of 5-phenyl-1H-indole-7-carboxamide (3.11 g, 12 mmol) in methanol (100 mL) was added benzyl piperidone (7.4 g, 36 mmol), followed by 156 mL of NaOMe (0.5 M in MeOH). The reaction mixture was then heated at 80° C. overnight. The solution was cooled to ambient temperature and the solvent removed under reduced pressure, and the resulting residue redisolved in a bilayer of ethyl acetate and 5% sodium hydroxide solution. The organic phase washed with brine, dried over potassium carbonate, and the solvent removed under reduced pressure. The residue was purified by silica gel chromatography (CH2Cl2:MeOH:NH4OH=96:3:1) to provide the desired product (2.66 g, 51%).

WORKUP

后处理

  1. temperatureThe solution was cooled to ambient temperature
  2. customthe solvent removed under reduced pressure
  3. washThe organic phase washed with brine
  4. dry with materialdried over potassium carbonate
  5. customthe solvent removed under reduced pressure
  6. customThe residue was purified by silica gel chromatography (CH2Cl2:MeOH:NH4OH=96:3:1)