HRID1280852

反应详情

EQUATION

反应方程式

HRID 1280852 的结构方程式

PROCEDURE

实验过程

2-Iodo-5-methylphenylacetic acid (20.0 g, 72 mmol) and a catalytic amount of 98% sulfuric acid (0.2 ml) are dissolved in isopropyl alcohol (200 ml) and heated to reflux temperature for 48 hours. The solvent is removed on a rotovap and the residual oil partitioned between EtOAc (500 ml) and saturated NaHCO3 solution (500 ml). The organic layer is separated, dried (MgSO4) and concentrated on a rotovap. The residual oil is distilled using a kugelrohr apparatus to give a clear, colorless oil which solidifies on standing at room temperature to give isopropyl 2-iodo-5-methylphenylacetate, m.p. 48-50°.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux temperature for 48 hours
  3. customThe solvent is removed on a rotovap
  4. customthe residual oil partitioned between EtOAc (500 ml) and saturated NaHCO3 solution (500 ml)
  5. customThe organic layer is separated
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated on a rotovap
  8. distillationThe residual oil is distilled
  9. customto give a clear, colorless oil which
  10. customon standing at room temperature