HRID2199512

反应详情

EQUATION

反应方程式

HRID 2199512 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A solution of (2R,3R)-butane-2,3-diol in THF was admixed at room temperature with potassium tert-butylate and the mixture was refluxed for 15 minutes. The mixture was cooled to ca. 50° C. and admixed with benzyl bromide. The mixture was refluxed for 3 hours, then stirred overnight at room temperature. The mixture was diluted with acetic ester and sodium chloride solution and then washed with 1 N hydrogen chloride solution (1×) and sodium chloride solution (2×). The organic phase was dried (Na2SO4), filtered and concentrated by evaporation. The residue obtained was purified by means of chromatography (hexane/acetic ester 1:1) (yield: 43%).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 15 minutes
  2. temperatureThe mixture was refluxed for 3 hours
  3. washwashed with 1 N hydrogen chloride solution (1×) and sodium chloride solution (2×)
  4. dry with materialThe organic phase was dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation
  7. customThe residue obtained
  8. customwas purified by means of chromatography (hexane/acetic ester 1:1) (yield: 43%)