HRID277989

反应详情

EQUATION

反应方程式

HRID 277989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Methoxy-5-Nitro-6-(2-Dimethylaminoethen-1-yl)pyridine (38.78 g, 174 mmol) was dissolved in 1.2 L of ethanol, and charged with 10% palladium on carbon (5.0 g). The mixture was hydrogenated at room temperature under 40 p.s.i. of hydrogen pressure for 4 hours. After filtration through celite followed by chromatography on silica gel (50% ethyl acetate/hexane), the material was recrystallized from ethyl acetate/hexane to provide 19.62 g of the title compound. (76%). MS(m/e): 149 (M+). EA calculated for C8H8N2O: C, 64.85; H, 5.44; N, 18.91. Found: C, 64.72; H, 5.33; N, 18.76.

WORKUP

后处理

  1. customwas hydrogenated at room temperature under 40 p.s.i
  2. filtrationAfter filtration through celite
  3. customthe material was recrystallized from ethyl acetate/hexane