HRID1893081

反应详情

EQUATION

反应方程式

HRID 1893081 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-[4-(methoxymethylene)cyclohexyl]-4-[2-(4-propylcyclohexyl)ethyl]-benzene (1.23 g, 2.74 mmol) was refuxed by a mixture of THF and 2N HCl (10 ml) in a volume ratio of 4:1. After reaction termination, the resulting solution was diluted by distilled water (10 ml), extracted by ether extraction (5 ml×2 times), and washed by distilled water (5 ml×2 times). The residue was purified by column chromatography (ethyl acetate:petroleum ether=1:60). The ratio of cis or trans-isomer of the obtained crystal was 1:5 with NMR analysis. The crystal was performed by fractional recrystallization with hexane to obtain pure trans-4-{4-[2-(4-propylcyclohexyl)ethyl]phenyl}cyclohexane carbaldehyde (0.2 g, 18%).

WORKUP

后处理

  1. customAfter reaction termination
  2. additionthe resulting solution was diluted
  3. distillationby distilled water (10 ml)
  4. extractionextracted by ether extraction (5 ml×2 times)
  5. washwashed
  6. distillationby distilled water (5 ml×2 times)
  7. customThe residue was purified by column chromatography (ethyl acetate:petroleum ether=1:60)
  8. customThe crystal was performed by fractional recrystallization with hexane