HRID841893

反应详情

EQUATION

反应方程式

HRID 841893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.2 g of 97 and 3.92 ml of perfluorobutyl iodide in 40 ml of diethyl ether are introduced under argon and methyllithium/lithium bromide complex (1.5 M in diethyl ether) is added in drops at −78° C. After 30 minutes, it is quenched with sodium chloride solution and diluted with ethyl acetate. Extraction with ethyl acetate, washing of the combined organic phases with sodium chloride solution, drying on sodium sulfate, removal of the solvent and chromatography on silica gel with ethyl acetate/hexane yields 2.1 g of 1-(2-methyl-1,3-dioxolan-2-yl)-α-(1,1,2,2,3,3,4,4,4-nonafluorobutyl)cyclopropanemethanol 98 as a colorless oil.

WORKUP

后处理

  1. customit is quenched with sodium chloride solution
  2. additiondiluted with ethyl acetate
  3. extractionExtraction with ethyl acetate
  4. washwashing of the combined organic phases with sodium chloride solution
  5. dry with materialdrying on sodium sulfate, removal of the solvent and chromatography on silica gel with ethyl acetate/hexane