In a 500ml single-necked round-bottom flask equipped with a magnetic stirrer and a reflux condenser, add 44.304g (0.213mol) of ω-acetoxymethyl camphene and 29.85g (0.533mol) of potassium hydroxide and dissolve it Distilled water, dropwise add to ω-acetoxymethyl camphene, then add 160ml of absolute ethanol, stir the reaction at room temperature (generally refers to 28-300C) for 18h, after the reaction is completed, transfer the reaction solution to a 1000ml beaker, add 200ml In ice water, and extracted with 3 * 25ml of petroleum ether, the organic phase was washed with distilled water until neutral, and the aqueous layer was separated. The oil layer was dried over anhydrous sodium sulfate, filtered, and transferred to a 150ml round bottom flask for rotary evaporation to remove petroleum ether , After refrigerated for several hours, a light yellow waxy solid can be obtained, and then the target product is recrystallized with petroleum ether. After drying, it can be weighed to obtain 25 g of white needle-like crystals (ie, ω-hydroxymethyl long leafene). The product has a purity of 99% by GC analysis and a yield of 49.59%
正在翻译中..