HRID1690193

反应详情

EQUATION

反应方程式

HRID 1690193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Ethyl 6-hydroxynicotinate (2.0 g, 12.0 mmol) was dissolved in pyridine (60 mL), which was then added with iodide (6.07 g, 23.9 mmol) and stirred at 60° C. overnight. The reaction solution was then added with water at room temperature and extracted with ethyl acetate. Subsequently, the organic layer was washed with a saturated aqueous solution of sodium sulfite and brine, and dried over sodium sulfate. The obtained residue was purified using column chromatography (chloroform/methanol) and concentrated in vacuo. Ethyl 6-hydroxy-5-iodonicotinate (2.9 g, yield 83%) was obtained as a yellow oil.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washSubsequently, the organic layer was washed with a saturated aqueous solution of sodium sulfite and brine
  3. dry with materialdried over sodium sulfate
  4. customThe obtained residue was purified
  5. concentrationconcentrated in vacuo