HRID1047900
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturerefluxed for 48 h
- customAfter removal of the EtOH in vacuo
- additionthe residue is diluted with water (125 mL)
- extractionextracted with EtOAc (3×75 mL)
- washThe organic extracts are washed with water (2×50 mL) and brine (2×50 mL)
- dry with materialdried over MgSO4
- concentrationConcentrated in vacuo