HRID408554

反应详情

EQUATION

反应方程式

HRID 408554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

100 mg (1.026 mmol) cyclopentane-1,3-dione, 150 mg (1.026 mmol) 1H-indazole-5-carbaldehyde and piperidine (0.1 ml) in ethanol (8 ml) were heated to reflux for 4 h. The mixture was then evaporated to dryness, the remaining solid was dissolved in acetic acid (8 ml), and 84 mg (1.026 mmol) 3-aminobut-2-enenitrile were added. The solution was heated to reflux for 2 h. After cooling, the mixture was evaporated to dryness again, and the remaining solid was purified by preparative RP-HPLC (acetonitrile/water gradient) to yield 40 mg (13% of th.) of the title compound.

WORKUP

后处理

  1. temperatureto reflux for 4 h
  2. customThe mixture was then evaporated to dryness
  3. dissolutionthe remaining solid was dissolved in acetic acid (8 ml)
  4. temperatureThe solution was heated
  5. temperatureto reflux for 2 h
  6. temperatureAfter cooling
  7. customthe mixture was evaporated to dryness again
  8. customthe remaining solid was purified by preparative RP-HPLC (acetonitrile/water gradient)