HRID646724

反应详情

EQUATION

反应方程式

HRID 646724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A slurry of 2-amino-5-bromopyridine-3-carboxylic acid (7 g, 32.2 mmol) in methanol (150 mL) and H2SO4 (7 mmol) was heated to reflux for 48 h. The reaction mixture was concentrated to ca. 40 mL. Water (100 mmol) was added to the residual oil, and the mixture neutralized with sodium carbonate. Ethyl acetate (400 mL) was added and the organic layer was washed with saturated aqueous sodium chloride then dried (Na2SO4) and concentrated to give the title compound (5.5 g, 73.9% yield).

WORKUP

后处理

  1. temperatureto reflux for 48 h
  2. concentrationThe reaction mixture was concentrated to ca. 40 mL
  3. washthe organic layer was washed with saturated aqueous sodium chloride
  4. dry with materialthen dried (Na2SO4)
  5. concentrationconcentrated