HRID487268

反应详情

EQUATION

反应方程式

HRID 487268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium metal (0.21 g, 9.2 mmol) was dissolved in ethanol (25 ml) and 6-carboethoxyimidazo[1,2-a]pyridine (1.75 g, 9.2 mmol) and 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide (1.02 g, 4.6 mmol) were added. The reaction mixture was heated to reflux for 24 hours, cooled to room temperature and stirred for 60 hours. The solvent was removed in vacuo, the residue was dissolved in water (100 ml) and the solution was neutralized by the addition of concentrated HCl. A precipitate was obtained which was collected by filtration through a glass frit. The solid was recrystallized from ethanol and washed with ether to afford 0.98 g (62%) of 1-cyclopentyl-3-ethyl-6-(6-imidazo[1,2-a]pyridinyl)-pyrazolo[3,4-d]pyrimidin-4-one as white crystals, m.p. >300° C. when dried for 18 hours at 120° C. in high vacuum.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 24 hours
  3. customThe solvent was removed in vacuo
  4. dissolutionthe residue was dissolved in water (100 ml)
  5. additionthe solution was neutralized by the addition of concentrated HCl
  6. customA precipitate was obtained which
  7. filtrationwas collected by filtration through a glass frit
  8. customThe solid was recrystallized from ethanol
  9. washwashed with ether