HRID1583650

反应详情

EQUATION

反应方程式

HRID 1583650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

One gram (6.5 mmol) of 2-methoxy-3-nitropyridine and 5.0 g (65 mmol) of ammonium acetate were added to a 100 ml round bottom flask. The reaction mixture was heated at 150° C. for approximately 16 hours under an argon atmosphere. An additional 5 g of ammonium acetate was added to the reaction mixture which was allowed to heat for an additional 8 hours. Thin layer chromatography of the mixture indicated that both product and starting material were present. The reaction mixture was cooled and poured into approximately 100 ml of water. The precipitated solid was collected by filtration to provide 209.8 mg of 3-nitro-2-aminopyridine. m/e 139. The NMR spectrum of the collected produot was identical to that of an authentic reference standard.

WORKUP

后处理

  1. temperatureto heat for an additional 8 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationThe precipitated solid was collected by filtration