HRID1893081
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAfter reaction termination
- additionthe resulting solution was diluted
- distillationby distilled water (10 ml)
- extractionextracted by ether extraction (5 ml×2 times)
- washwashed
- distillationby distilled water (5 ml×2 times)
- customThe residue was purified by column chromatography (ethyl acetate:petroleum ether=1:60)
- customThe crystal was performed by fractional recrystallization with hexane