HRID269584

反应详情

EQUATION

反应方程式

HRID 269584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Chloro-3-pyridinol (2.0 g, 15.44 mmol) was stirred in water (40 ml) containing sodium carbonate (3.43 g, 32.36 mmol) and iodine (3.92 g, 15.44 mmol) was added. The mixture was stirred at room temperature for 72 hours. The pH was adjusted to pH8 with 1M hydrochloric acid solution and the mixture extracted with ethyl acetate (×2). The combined organic extracts were washed with brine and dried (MgSO4). The aqueous layer was acidified to pH5 with 1M hydrochloric acid solution and extracted with ethyl acetate, which was washed with brine, dried (MgSO4) and the combined solutions evaporated to leave the title compound as a buff solid (3.70 g).

WORKUP

后处理

  1. additionwas added
  2. extractionthe mixture extracted with ethyl acetate (×2)
  3. washThe combined organic extracts were washed with brine
  4. dry with materialdried (MgSO4)
  5. extractionextracted with ethyl acetate, which
  6. washwas washed with brine
  7. dry with materialdried (MgSO4)
  8. customthe combined solutions evaporated