HRID523098

反应详情

EQUATION

反应方程式

HRID 523098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 6-bromo-2-methoxypyridin-3-amine (96 mg, 0.473 mmol), 1,2-dimethyl-1H-imidazole (91 mg, 0.946 mmol), Pd(OAc)2 (4.3 mg, 0.019 mmol), KOAc (93 mg, 0.95 mmol) in DMA (3 mL) was stirred at 1500 under microwave irradiation for 8 hours. The reaction mixture was filtered, diluted with NaCl solution and extracted with EtOAc. The organic layer was purified by eluting through an SCX-2 column using 2M NH3/MeOH followed by Biotage silica gel column chromatography eluting with 0-4% MeOH/EtOAc to give the title compound as pink solid (17 mg, 16%).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. additiondiluted with NaCl solution
  3. extractionextracted with EtOAc
  4. customThe organic layer was purified
  5. washby eluting through an SCX-2 column
  6. washeluting with 0-4% MeOH/EtOAc