HRID516861

反应详情

EQUATION

反应方程式

HRID 516861 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2-(3-methoxy-4-methylphenyl)acetic acid (Step A, 4.64 g, 25.7 mmol) in ethanol (100 ml) was added p-TsOH (0.7 g, 3.7 mmol) at room temperature under argon and the reaction mixture was refluxed for 12 hours or until all the starting material is consumed, concentrated, diluted in EtOAc and washed with 0.1N HCl, brine, dried over Na2SO4, filtered, concentrated and purified by flash chromatography on a silica gel column (hexane:ethyl acetate, 2:1) to give the title compound.

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 12 hours or until all the starting material
  2. customis consumed
  3. concentrationconcentrated
  4. additiondiluted in EtOAc
  5. washwashed with 0.1N HCl, brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. custompurified by flash chromatography on a silica gel column (hexane:ethyl acetate, 2:1)