HRID496594

反应详情

EQUATION

反应方程式

HRID 496594 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1.268 g (5 mmol) of ethyl 4-chloro-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate and 7.5 ml (15 mmol) of methylamine in tetrahydrofuran (2.0 molar solution) was stirred at room temperature overnight and refluxed for 2 hours. The solvent was removed to give a white solid. The solid was dissolved in ethyl acetate and the solution washed with H2O, 1M NaHCO3, brine and dried (Na2SO4). The solvent was removed to give a white solid. Crystallization from ethyl acetate gave 0.715 g of white solid; Mass spectrum (ES) 249.2 (M+H).

WORKUP

后处理

  1. temperaturerefluxed for 2 hours
  2. customThe solvent was removed
  3. customto give a white solid
  4. washthe solution washed with H2O, 1M NaHCO3, brine
  5. dry with materialdried (Na2SO4)
  6. customThe solvent was removed
  7. customto give a white solid
  8. customCrystallization from ethyl acetate