HRID1597841

反应详情

EQUATION

反应方程式

HRID 1597841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium spheres (207 mg) was dissolved in ethanol (15 ml) and 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide (1 g, 45 mmol) was added, followed by ethyl 2-(2-propenyloxy)benzoate (1.85 g, 9 mmol). The reaction mixture was refluxed overnight, cooled, the ethanol was stripped and water was added. The pH was adjusted to about 7 and a solid was isolated by filtration. The solid was taken up in ether, washed with dilute HCl, dried over MgSO4, filtered and the solvent was removed and the solid residue was recrystallized from ether to afford 0.56 g of 1-cyclopentyl-3-ethyl-6-[2-(CH2 =CH--CH2 O)phenyl]pyrazolo[3,4-d]pyrimidin-4-one, m.p. 119°-120° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed overnight
  2. temperaturecooled
  3. customa solid was isolated by filtration
  4. washwashed with dilute HCl
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customthe solvent was removed
  8. customthe solid residue was recrystallized from ether