Biopharmaceutical Raw Materials CAS 24324-17-2 9-fluorenylmethanol

9-Fluorenylmethanol(CAS NO 24324-17-2)

Specifications:

Preparation of  9-fluorenylmethanol

 9-fluorenylmethanol CAS NO 24324-17-2,the preparation of  9-fluorenylmethanolWeigh 83.0g industrial fluorene into a 1000ml four-necked flask, add dichloromethane, ethyl formate, and then NaH, stir and heat to reflux for 12h, slowly pour the reaction solution into 1000g ice water, stir, layer, separate the organic phase , Recovery of dichloromethane and excess ethyl formate. The water layer was washed twice with petroleum ether and then neutralized by adding glacial acetic acid. The solution gradually thickened until a large amount of solids appeared. Dichloromethane was added to dissolve the solids. The organic phase was collected. The water layer was extracted twice with dichloromethane and the organic phases were combined. Then wash the organic phase with saturated NaHCO3, heat the dichloromethane with anhydrous sodium sulfate, add 400ml methanol, slowly add 17g potassium borohydride to the ice solution, stir for 2.5h, pour into 4L ion exchange water, stir, slowly Add 150ml of glacial acetic acid to neutralize to obtain a pale yellow precipitate, that is, the crude product, which is filtered with suction, washed with water, decolorized, recrystallized, and dried to obtain white needle-like crystals of fluorene methanol, with a melting point of 101~102°C and a liquid chromatography content of 99.98%  9-fluorenylmethanol.

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