HRID2087049
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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. 48-500.
WORKUP
后处理
- temperatureheated
- temperatureto reflux temperature for 48 hours
- customThe solvent is removed on a rotovap
- customthe residual oil partitioned between EtOAc (500 ml) and saturated NaHCO3 solution (500 ml)
- customThe organic layer is separated
- dry with materialdried (MgSO4)
- concentrationconcentrated on a rotovap
- distillationThe residual oil is distilled
- customto give a clear, colorless oil which
- customon standing at room temperature