HRID1047900

反应详情

EQUATION

反应方程式

HRID 1047900 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of the 2-iodo-3-methylbenzoic acid (6 g-0.023 mol) in EtOH (150 mL) is treated with concentrated HCl (20 mL) and refluxed for 48 h. After removal of the EtOH in vacuo, the residue is diluted with water (125 mL) and cooled to 0° C. in an ice bath. The pH is adjusted to 10 with solid NaOH pellets and extracted with EtOAc (3×75 mL). The organic extracts are washed with water (2×50 mL) and brine (2×50 mL) and dried over MgSO4. Concentrated in vacuo to give the product as a pale yellow oil. (6 g, 90%).

WORKUP

后处理

  1. temperaturerefluxed for 48 h
  2. customAfter removal of the EtOH in vacuo
  3. additionthe residue is diluted with water (125 mL)
  4. extractionextracted with EtOAc (3×75 mL)
  5. washThe organic extracts are washed with water (2×50 mL) and brine (2×50 mL)
  6. dry with materialdried over MgSO4
  7. concentrationConcentrated in vacuo