HRID1095244

反应详情

EQUATION

反应方程式

HRID 1095244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound (17) was dissolved in a mixed solvent of toluene (150 ml) and Solmix (150 ml) and 3.48 g of Pd/C was added thereto. The mixture was stirred at room temperature under a hydrogen atmosphere until hydrogen absorption had ceased. After the reaction had been completed, Pd/C was removed and then the solvent was distilled off. The residue was purified with a fractional operation by means of column chromatography using a mixed solvent of toluene and ethyl acetate (toluene:ethyl acetate=9:1 by volume) as an eluent and silica gel as a stationary phase powder and dried, giving 61.9 g of 8-(3-fluorophenyl)-1,4-dioxaspiro[4,5]decane (18). The yield based on the compound (17) was 88.1%.

WORKUP

后处理

  1. additionwas added
  2. customPd/C was removed
  3. distillationthe solvent was distilled off
  4. customThe residue was purified with a fractional operation by means of column chromatography
  5. customsilica gel as a stationary phase powder and dried