HRID1199962

反应详情

EQUATION

反应方程式

HRID 1199962 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7.8 g. (35 mmole) 4-chloro-1-(tetrahydrofuran-2-yl)-1H-pyrazolo[3,4-d]pyrimidine, 20.3 g. (100 mmole) N-(2,5-dimethylbenzyl)-cyclopentylamine and 100 ml. n-butanol is heated under reflux for 16 hours. The reaction mixture is evaporated, the residue is taken up in water and extracted with dichloromethane and the extract is washed with dilute acetic acid and dilute aqueous sodium hydrogen carbonate solution, dried, evaporated and chromatographed on silica gel. 5.0 g. (37% of theory) of the title compound are eluted with dichloromethane/methanol (98:2 v/v) which, after trituration with diethyl ether, melts at 173°-174° C.

WORKUP

后处理

  1. additionA mixture of 7.8 g
  2. temperatureunder reflux for 16 hours
  3. customThe reaction mixture is evaporated
  4. extractionextracted with dichloromethane
  5. washthe extract is washed with dilute acetic acid and dilute aqueous sodium hydrogen carbonate solution
  6. customdried
  7. customevaporated
  8. customchromatographed on silica gel
  9. wash(37% of theory) of the title compound are eluted with dichloromethane/methanol (98:2 v/v) which