Preparation method of dihydroxy oxethyl fluorene
A technology of bishydroxyethoxyfluorene and fluorenone, which is applied in the field of preparation of bishydroxyethoxyfluorene, can solve the problems of long reaction time, high reaction temperature, and increased cost, and achieve improved crystal form, fluidity, and process Simplified operation and beneficial effect of recycling
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Embodiment 1
[0020] Example 1: Synthesis of BPEF.
[0021] Add 18g of fluorenone (0.1mol) with a content of 99% or more (HPLC), 50g of ethylene glycol monophenyl ether (0.36mol) with a content of 99% or more (GC), and 1g of mercaptoethanol (0.0128mol) in a 250ml flask. Stir for 0.5 hours, then add 35g of concentrated sulfuric acid with a content of 98% dropwise at 65-70°C within 3 hours. The combined organic layers were extracted twice with hydrocarbons, cooled to 0-5°C, crystallized, filtered and dried to obtain 41g of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, with a yield of 93.5%, and a content of 98.2 %about.
Embodiment 2
[0022] Example 2: Synthesis of BPEF.
[0023] Add 18g of fluorenone (0.1mol) with a content of 99% or more (HPLC), 45g of ethylene glycol monophenyl ether (0.36mol) with a content of 99% or more (GC), and 0.9g of mercaptoethanol in a 250ml flask. Stir for 0.5-2 hours, then add 37g of concentrated sulfuric acid with a content of 98% dropwise at 60-70°C within 2.5 hours. The combined organic layer was extracted twice with alkanes and other halogenated hydrocarbons, cooled to 0-5°C, crystallized, filtered and dried to obtain 42g of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, with a yield of 95.7% , the content is about 98.4%.
Embodiment 3
[0024] Example 3: Purification of BPEF.
[0025] Get 20g of the product obtained in Example 2, recrystallize twice with 60ml of ethylene dichloride, and filter and dry to obtain 18.8g of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, with a purity of 99.8%.
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