HRID1926588

反应详情

EQUATION

反应方程式

HRID 1926588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 2-methylsulfonyl-4-(pyridin-3-yl)pyrimidine (3.0 g) and 2-methyl-3-amino-5-nitropyridine (5.0 g) in DMF (50 mL) at 0-5° C. was added sodium hydride (60%, 2.3 g). The reaction mixture was naturally warmed to room temperature and stirred for 6 hours. Chloroform (50 mL) and water (50 mL) were added to the reaction and the phases were separated, the aqueous phase was extracted with Chloroform (2×100 mL). The organic extracts were combined, dried, filtered, concentrated and the residue was purified by chromatography to provide_N-(5-nitro-2-methylpyrid-3-yl)-4-(pyrid-3-yl)-2-pyrimidinamine (5.2 g).

WORKUP

后处理

  1. customthe phases were separated
  2. extractionthe aqueous phase was extracted with Chloroform (2×100 mL)
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customthe residue was purified by chromatography to provide_N-(5-nitro-2-methylpyrid-3-yl)-4-(pyrid-3-yl)-2-pyrimidinamine (5.2 g)