HRID619165

反应详情

EQUATION

反应方程式

HRID 619165 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a slurry of 1-cyclopentyl-3-ethyl-6-[3-(ethoxycarbonylmethoxy)phenyl]pyrazolo[3,4-d]pyrimidin-4-one (1.23 g, 3.0 mmol) in ethanol (10 ml) was added water (100 ml), followed by 85% KOH (0.4 g). The reaction mixture was heated on a steam bath for 3 hours, cooled to room temperature and filtered. The filtrate was chilled and acidified with acetic acid to afford a white precipitate, which was collected by filtration and washed with water, then ethanol, and finally ether. The product was combined with the product from another experimental run and then was recrystallized from DMF/CH3CN to afford 0.98 g of 1-cyclopentyl-3-ethyl-6-[3-(carboxymethoxy)phenyl]pyrazolo[3,4-d]pyrimidin-4-one, m.p. 299-300° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated on a steam bath for 3 hours
  2. filtrationfiltered
  3. temperatureThe filtrate was chilled
  4. customto afford a white precipitate, which
  5. filtrationwas collected by filtration
  6. washwashed with water
  7. customwas recrystallized from DMF/CH3CN