HRID487259

反应详情

EQUATION

反应方程式

HRID 487259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

1-Cyclopentyl-3-ethyl-6-(4-quinolinyl)-pyrazolo[3,4-d]-pyrimidin-4-one (1.0 g, 2.7 mmol), platinum oxide (0.15 g) and acetic acid (50 ml) were combined and placed in a parr hydrogenator at 42 psi. The reaction mixture was heated at about 70° C. by an external heating jacket for 6 hours. The reaction mixture was cooled to room temperature, the catalyst was removed by filtration through a celite pad and the pad was washed with ethanol. Concentrated HCl (3 ml) was added to the filtrate and the solvents were removed in vacuo. The residue was dissolved in isopropanol (10 ml) and was heated on a steam bath for 10 minutes. A solid was collected by filtration, washed with isopropanol and dried at 90° C. in high vacuum to afford 0.83 g (84%) of 1-cyclopentyl-3-ethyl-6-(perhydro-4-quinolinyl)pyrazolo[3,4-d]pyrimidin-4-one as a white powder, m.p. >300° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customthe catalyst was removed by filtration through a celite pad
  3. washthe pad was washed with ethanol
  4. additionConcentrated HCl (3 ml) was added to the filtrate
  5. customthe solvents were removed in vacuo
  6. dissolutionThe residue was dissolved in isopropanol (10 ml)
  7. temperaturewas heated on a steam bath for 10 minutes
  8. filtrationA solid was collected by filtration
  9. washwashed with isopropanol
  10. customdried at 90° C. in high vacuum