HRID639042

反应详情

EQUATION

反应方程式

HRID 639042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Ethyl(6-bromo-2-nitro-pyridin-3-yloxy)acetate (38 g, 0.125 mole) was dissolved in glacial AcOH (150 mL), and iron powder (20 g, 0.36 mole) was added. The mixture was mechanically stirred and heated at 90° C. for 5 hr, then was cooled to room temperature and diluted with EtOAc (300 mL). The mixture was filtered through a pad of silica gel and the filtrate was concentrated in vacuo and the residue recrystallized from MeOH (15 g, 52%); MS (ES) m/z 229.0 (M+H)+.

WORKUP

后处理

  1. temperaturewas cooled to room temperature
  2. filtrationThe mixture was filtered through a pad of silica gel
  3. concentrationthe filtrate was concentrated in vacuo
  4. customthe residue recrystallized from MeOH (15 g, 52%)