HRID481308

反应详情

EQUATION

反应方程式

HRID 481308 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6-chloro-2-pyridinecarboxylic acid (14.8 g, 0.093 mol, for preparation, see Delarge, II. Farmaco-Ed.Sc., 1967, 22, 1069) in trifluoroacetic acid (110 ml) was added 75 ml of 30% aqueous hydrogen peroxide solution. The mixture was heated to 60° for 2 hours, cooled to room temperature and poured onto ice water. The white precipitate was filtered and was washed well with water to yield 10.8 g (67%) of the title compound of this preparation. mp 168°-170° C. 1H NMR (CDCl3): δ 7.46 (1H, d, J=8), 7.77 (1H, dd, J=8, 8), 8.01 (1H, d, J=8).

WORKUP

后处理

  1. temperatureThe mixture was heated to 60° for 2 hours
  2. additionpoured onto ice water
  3. filtrationThe white precipitate was filtered
  4. washwas washed well with water
  5. customto yield