HRID2219584

反应详情

EQUATION

反应方程式

HRID 2219584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.00 g (12.04 mmol) 3-Amino-pyridine-2-carboxylic acid ethyl ester and 2.57 g (14.44 mmol, 1.2 equiv.) of N-Bromosuccinimide in 80 ml of acetonitrile was stirred for 2 h at room temperature. Silicagel (5 g) was added to the reaction mixture Which was evaporated to dryness. The residue was loaded onto a Flash chromatography column (SiO2, 50 g) and eluted with heptane/ethyl acetate 3:1. One obtains 1.11 g (4.51 mmol, 37%) of the title compound as a white cristalline solid, MS (ISP): m/e=245.1, 247.1 (M+H+).

WORKUP

后处理

  1. additionSilicagel (5 g) was added to the reaction mixture Which
  2. customwas evaporated to dryness
  3. washeluted with heptane/ethyl acetate 3:1