HRID1366517

反应详情

EQUATION

反应方程式

HRID 1366517 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Commercially available N-methyl-1-(4-pyridinyl)methanamine (0.305 g, 2.5 mmol) was dissolved in THF (5 mL). To this solution was added triethylamine (0.38 mL, 2.73 mmol), followed by 2,4,6-trichloro-5-fluoropyrimidine (0.5 g, 2.5 mmol), which was dissolved in THF (5 mL). The reaction was left to stir for 2.5 hours. The reaction mixture was diluted with water, then extracted with ether. The organics were dried (MgSO4) and concentrated. The resulting material was purified via filtration over silica gel with a solvent mixture of 5% MeOH in 95% DCM as the mobile phase to provide 2,6-dichloro-5-fluoro-N-methyl-N-(4-pyridinylmethyl)-4-pyrimidinamine as a brown oily solid (0.3516 g, 49%). LCMS: (M+H)+=287.0.

WORKUP

后处理

  1. waitThe reaction was left
  2. extractionextracted with ether
  3. dry with materialThe organics were dried (MgSO4)
  4. concentrationconcentrated
  5. filtrationThe resulting material was purified via filtration over silica gel with a solvent mixture of 5% MeOH in 95% DCM as the mobile phase