HRID40897

反应详情

EQUATION

反应方程式

HRID 40897 的结构方程式

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 4-(1H-pyrazol-4-yl)-7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]-pyrimidine (0.216 g, 0.684 mmol) in ACN (4 mL, 0.08 mol) was added crude senecionitrile (0.111 g, 1.37 mmol), followed by DBU (200 μL, 0.002 mol) and the resulting mixture was heated to 60° C. for 23 hours. The mixture was cooled to room temperature and the ACN was evaporated. The mixture was diluted with ethyl acetate and washed with dilute HCl and brine. The organic solution was dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography (ethyl acetate/hexanes) afforded the desired product.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. customthe ACN was evaporated
  3. additionThe mixture was diluted with ethyl acetate
  4. washwashed with dilute HCl and brine
  5. dry with materialThe organic solution was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customPurification by silica gel chromatography (ethyl acetate/hexanes)