HRID1027848

反应详情

EQUATION

反应方程式

HRID 1027848 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

3.82 g (20.0 mmol) of copper(I) iodide, 0.97 g (16.7 mmol) of potassium fluoride and 2.47 ml (16.7 mmol) (trifluoromethyl)-trimethylsilane were added, with stirring, to a solution of 4.66 g (11.1 mmol) of 4-((1R,2R)-2-benzyloxy-1-methyl-propoxy)-2-chloro-5-iodo-pyrimidine in 15.8 ml NMP and 15.8 ml THF at room temperature. The mixture was stirred for 5.5 hours at 80° C. After cooling, the mixture was added to dilute sodium chloride solution and was extracted with ethyl acetate (2×). The combined organic phases were dried (Na2SO4), filtered and concentrated by evaporation. The residue obtained was chromatographically (hexane/ethyl acetate 4:1). 2.17 g (6.0 mmol; yield: 54%) of the product was obtained.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionwas extracted with ethyl acetate (2×)
  3. dry with materialThe combined organic phases were dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated by evaporation
  6. customThe residue obtained
  7. custom2.17 g (6.0 mmol; yield: 54%) of the product was obtained