HRID2223869

反应详情

EQUATION

反应方程式

HRID 2223869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of [2-[1-[2-(tert-butyldiphenylsiloxy)ethyl]cyclohexyl]ethanol (1.25 g) dissolved in benzene (15 mL) were added acetone cyanohydrin (0.40 mL), tri-n-butylphosphine (1.08 mL) and 1,1-azobis(N,N-dimethylformamide) (754 mg). The solution was stirred at room temperature for 18 hours. The solvent was distilled off under reduced pressure, ethyl acetate was added and insolubles were filtered off. The solvent was distilled off under reduced pressure. The resulting residue was purified by column chromatography (silica gel, hexane:ethyl acetate=5:1) to give the title compound (1.07 g).

WORKUP

后处理

  1. distillationThe solvent was distilled off under reduced pressure, ethyl acetate
  2. additionwas added
  3. filtrationinsolubles were filtered off
  4. distillationThe solvent was distilled off under reduced pressure
  5. customThe resulting residue was purified by column chromatography (silica gel, hexane:ethyl acetate=5:1)