HRID271554

反应详情

EQUATION

反应方程式

HRID 271554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

1-Prop-2-ynyl-1H-imidazole (15 mmol) is dissolved in DMF at room temperature under nitrogen atmosphere. To the solution, 5-bromo-4-(2,2-dimethyl-propylamino)-pyrimidine-2-carbonitrile (8 mmol), triethylamine (24 mmol), copper(I) iodide (0.8 mmol), and dichlorobis(triphenylphosphine)palladium (II) (0.4 mmol) are added successively. The mixture is heated at 80° C. under nitrogen atmosphere for 3 h. After cooling at room temperature, the mixture is diluted with H2O and AcOEt and filtered with celite. The organic layer is taken, dried over MgSO4 and evaporated in vacuo. The residue is purified by silica gel column chromatography (AcOEt:MeOH=20:1) to give 7-(2,2-dimethyl-propyl)-6-imidazol-1-ylmethyl-7H-pyrrolo[2,3-d]pyrimidine-2-carbonitrile in 64% yield.

WORKUP

后处理

  1. temperatureAfter cooling at room temperature
  2. filtrationfiltered with celite
  3. dry with materialdried over MgSO4
  4. customevaporated in vacuo
  5. customThe residue is purified by silica gel column chromatography (AcOEt:MeOH=20:1)