HRID2268567

反应详情

EQUATION

反应方程式

HRID 2268567 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 3-bromo-5-hydroxybenzoic acid methyl ester (10.2 g) and tert-butyl bromoacetate (9.7 ml) in anhydrous DMF was added sodium hydride (60% dispersion in mineral oil, 2.69). After 30 min water (10 ml) aws added. The reaction mixture was partitioned between ethyl acetate and water. The aqueous phase was removed and the organic phase washed with further water, 1M sodium hydroxide solution and dried with brine and over sodium sulphate. Concentration under reduced pressure gave the title compound as dark yellow gum (12.8 g).

WORKUP

后处理

  1. customThe reaction mixture was partitioned between ethyl acetate and water
  2. customThe aqueous phase was removed
  3. washthe organic phase washed with further water, 1M sodium hydroxide solution
  4. dry with materialdried with brine and over sodium sulphate
  5. concentrationConcentration under reduced pressure