Refining of 9-fluorene methanol
1. Put the products obtained from multiple tests into a mortar and grind them evenly. Add the homogenized crude product to an appropriate amount of 1:1 ethanol aqueous solution (volume ratio), heat up to 60°C, then slowly cool the aqueous solution to room temperature, and then cool it in an ice water bath. Use a glass rod to continuously rub the wall of the cup until the crystals are complete. After precipitation, vacuum filtration, washing with a certain amount of water, and drying. 2. Add the crude product obtained in 1 to an appropriate amount of toluene and heat to about 90°C. After all the 9-fluorene methanol is dissolved, cool to room temperature, and then put the mixture in an ice bath to cool, while continuously using a glass rod Rub the wall of the cup with ground, and wait for the white needle-like crystals to completely precipitate out. After vacuum filtration and washing with a certain amount of water, white needle-like crystals of 9-fluorene methanol are obtained. According to high performance liquid chromatography analysis, the purity of 9-fluorene methanol is about 99.9%.
