HRID893418

反应详情

EQUATION

反应方程式

HRID 893418 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

60.9 g of methyl 3-[2,4-dimethoxy-5-(4-methoxybenzoyl)phenyl]propionate are mixed with 300 ml of 2N sodium hydroxide solution and 300 ml of dioxane and stirred overnight. The dioxane is then removed in vacuo, and the alkaline aqueous solution is extracted once with 100 ml of ethyl acetate. The aqueous phase is adjusted to pH 2 with concentrated hydrochloric acid, when part of the product separates out. The mixture is extracted three times with 200 ml of ethyl acetate each time, and the organic phase is washed with water, dried over sodium sulfate and concentrated. The residue is recrystallized from ethyl acetate/acetone/hexane.

WORKUP

后处理

  1. customThe dioxane is then removed in vacuo
  2. extractionthe alkaline aqueous solution is extracted once with 100 ml of ethyl acetate
  3. extractionThe mixture is extracted three times with 200 ml of ethyl acetate each time
  4. washthe organic phase is washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue is recrystallized from ethyl acetate/acetone/hexane