HRID656877

反应详情

EQUATION

反应方程式

HRID 656877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,7-bis(methoxy)-1,5-naphthyridine (7.45 g, 39.210 mmol) stirred in glacial acetic acid (100 ml) at rt under argon, was treated with 33% HBr in acetic acid (100 ml). After stirring at rt for 18 h, the solvents were evaporated under reduced pressure (copious fumes of HBr were produced). The orange solid residue was stirred with water (ca. 250 ml) and the pH of the suspension was adjusted to ca. pH 6 by addition of solid sodium hydrogen carbonate. The mixture was then filtered and dried in a vacuum desiccator over P2O5 overnight to give 7-(methoxy)-1,5-naphthyridin-2(1H)-one as an off-white solid (5.958 g, 86%).

WORKUP

后处理

  1. customthe solvents were evaporated under reduced pressure (copious fumes of HBr were produced)
  2. stirringThe orange solid residue was stirred with water (ca. 250 ml)
  3. additionthe pH of the suspension was adjusted to ca. pH 6 by addition of solid sodium hydrogen carbonate
  4. filtrationThe mixture was then filtered
  5. dry with materialdried in a vacuum desiccator over P2O5 overnight