HRID2257037

反应详情

EQUATION

反应方程式

HRID 2257037 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

To a solution of 1-cyclopentyl-3-ethyl-6-(3-methoxyphenylmethyl)pyrazolo[3,4-d]pyrimidin-4-one (4.49 g, 13 mmol) in DMF (123 mL) was added 97% NaH (1.26 g), followed 20 minutes later by propanethiol (2.96 g, 39 mmol). The reaction mixture was heated at 130° C. overnight, cooled to room temperature and then ice water, followed by acetic acid were added. A precipitate formed which was collected by filtration, recrystallized from ether and dried at 110° C. and 2 mm Hg to afford 2.72 g of 1-cyclopentyl-3-ethyl-6-(3-hydroxyphenylmethyl)pyrazolo[3,4-d]pyrimidin-4-one, m.p. 195°-197° C.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. additionwere added
  3. customA precipitate formed which
  4. filtrationwas collected by filtration
  5. customrecrystallized from ether
  6. customdried at 110° C.