HRID1027846

反应详情

EQUATION

反应方程式

HRID 1027846 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

5.00 g (44.6 mmol) of potassium tert.-butylate was added to a solution of 4.00 g (44.4 mmol) (2R,3R)-butane-2,3-diol in 300 ml THF at room temperature and the mixture was refluxed for 15 minutes. The mixture was cooled to approx. 50° C. and 5.3 ml (44.6 mmol) benzyl bromide was added. It was refluxed for 3 hours, and was then stirred overnight at room temperature. The mixture was diluted with ethyl acetate and sodium chloride solution and then washed with 1N 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 chromatographically (hexane/ethyl acetate 1:1). 3.41 g (18.9 mmol; yield: 43%) of the product was obtained.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 15 minutes
  2. temperatureIt was refluxed for 3 hours
  3. washwashed with 1N 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 chromatographically (hexane/ethyl acetate 1:1)
  9. custom3.41 g (18.9 mmol; yield: 43%) of the product was obtained