HRID928171

反应详情

EQUATION

反应方程式

HRID 928171 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of tert-butyl 3-(9-isopropyl-6-((1-methyl-1H-pyrazol-4-yl)amino)-9H-purin-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate (821 mg, 1.87 mmol) in ethanol (35 mL) was degassed with nitrogen and to this was added 10%-Pd/C (150 mg), and ammonium formate (650 mg, 10 mmol). The resulting mixture was stirred and heated at 60° C. for 3 hr. The reaction was cooled to ambient temperature and the catalyst was removed by filtration. The filtrate was evaporated to give a residue, which was taken into ethyl acetate (100 mL) and the solution washed with water (30 mL), brine (30 mL), dried over Na2SO4 and evaporated to give a residue that was purified via flash chromatography with a gradient from 100% heptane to 100% ethyl acetate to afford the title compound (620 mg), which was used in the following step.

WORKUP

后处理

  1. temperatureThe reaction was cooled to ambient temperature
  2. customthe catalyst was removed by filtration
  3. customThe filtrate was evaporated
  4. customto give a residue, which
  5. washthe solution washed with water (30 mL), brine (30 mL)
  6. dry with materialdried over Na2SO4
  7. customevaporated
  8. customto give a residue that
  9. customwas purified via flash chromatography with a gradient from 100% heptane to 100% ethyl acetate