HRID990909

反应详情

EQUATION

反应方程式

HRID 990909 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under an atmosphere of argon gas, to sodium methoxide (160 g), methanol (800 ml) was added with stirring. Thereto, a solution of 3-bromomethylphenylacetic acid (226 g; prepared in Reference Example 18) in methanol (3200 ml) was added. The mixture was refluxed for 20 minutes. After the temperature of mixture became to room temperature, methanol was distilled off. The residue was poured into 2N HCl. Thereto, ethyl acetate was added. The organic layer was washed by an aqueous saturated solution of sodium chloride, dried over anhydrous magnesium sulfate and concentrated to obtain the title compound (176.3 g).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 20 minutes
  2. custombecame to room temperature
  3. distillationmethanol was distilled off
  4. additionThe residue was poured into 2N HCl
  5. additionThereto, ethyl acetate was added
  6. washThe organic layer was washed by an aqueous saturated solution of sodium chloride
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated