HRID1943544

反应详情

EQUATION

反应方程式

HRID 1943544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound (9) (50.0 g) was dissolved in a mixed solvent of toluene (150 ml) and Solmix A-11 (150 ml), Pd/C (0.5 g) was added thereto, and 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 obtained was purified with a fractional operation by means of column chromatography using heptane as the eluent and silica gel as the stationary phase powder, and further purified by means of recrystallization from Solmix A-11 and dried, giving 47.0 g of 4-pentyl-(2,3-difluorophenyl)cyclohexane (10). The yield based on the compound (9) was 94.0%.

WORKUP

后处理

  1. additionwas added
  2. customPd/C was removed
  3. distillationthe solvent was distilled off
  4. customThe residue obtained
  5. customwas purified with a fractional operation by means of column chromatography
  6. customfurther purified by means of recrystallization from Solmix A-11
  7. customdried