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Preparation method of 9,9-fluorene diethanol

A technology of fluorene diethanol and ethylene oxide, applied in 9 fields, can solve the problems of high cost, low yield, complicated process and the like of the preparation method, and achieve the effects of remarkable technological progress, stable yield and optimized reaction temperature.

Active Publication Date: 2016-05-18
XUZHOU B&C CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the above-mentioned technical problems in the prior art, the invention provides a kind of preparation method of 9,9-fluorene diethyl alcohol, the preparation method of described this 9,9-fluorene diethanol solves the preparation method in the prior art Technical problems of high method cost, complex process and low yield

Method used

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  • Preparation method of 9,9-fluorene diethanol
  • Preparation method of 9,9-fluorene diethanol
  • Preparation method of 9,9-fluorene diethanol

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add the raw material fluorene (100g) to N,N-dimethylformamide (750ml), under nitrogen protection, stir until the solids are completely dissolved, cool to 0°C, add sodium hydride (60g, 3-4 times, 15 minutes to complete the addition), and maintain the temperature between 0 and 5°C (a large amount of gas is released). After the addition, the temperature in the reaction bottle was kept at 0-10°C. After stirring for one hour, it was cooled to 0°C again, and then ethylene oxide (60ml) was diluted with N,N-dimethylformamide (50ml). Add it to the reaction bottle (addition is completed in one minute), after the addition, slowly rise to 15°C, and keep it warm for 5 hours (in-control 1). Post-treatment, the reaction mixture was slowly poured into 800g of ice water to quench, then extracted with EA (ethyl acetate) (800ml×3), the organic phase was combined, and the organic phase was washed once with saturated brine (800ml), and sulfuric acid was added Sodium dry. After filtering o...

Embodiment 2

[0035] Add the raw material fluorene (60g) to N,N-dimethylformamide (450ml), under nitrogen protection, stir until the solids are completely dissolved, then cool to 0°C, add sodium hydride (36g, 3-4 times, 15 minutes to complete the addition), and maintain the temperature between 0 and 5°C (a large amount of gas is released). After the addition, the temperature in the reaction flask was kept at 0-10°C. After stirring for one hour, it was cooled to 0°C again, and then ethylene oxide (36ml) was diluted with N,N-dimethylformamide (30ml). Add it into the reaction bottle (addition is completed in one minute), after the addition is completed, slowly rise to 15°C, and keep it warm for 5 hours. After treatment, the reaction mixture was slowly poured into 480g of ice water to quench, and then extracted with EA (ethyl acetate) (480ml×3), the organic phase was combined, and the organic phase was washed once with saturated brine (480ml), and sulfuric acid was added Sodium dry. After fil...

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Abstract

The invention provides a preparation method of 9,9-fluorene diethanol. Firstly, fluorene, ethylene oxide, sodium hydride and N,N-dimethyl formamide are weighed according to the material proportion, the raw material fluorine is added into the N,N-dimethyl formamide, stirring is performed under the nitrogen protection till the mixture is completely dissolved, then cooling is performed, the sodium hydride is added in batches, the temperature is kept to be 0-5 DEG C, stirring is performed for reaction, and then the epoxy ethane is diluted by using the N,N-dimethyl formamide and then is added into a reaction container to perform heat preservation reaction; the reaction mixture is added into ice water for quenching, extraction is performed by using ethyl acetate, organic phases are mixed, washing and drying are performed, water bath is performed after a desiccant is filtered out, activated carbon is added for reflux and decoloration, and the solvent is spin-dried to obtain a coarse product after the activated carbon is filtered out; the crude product is dissolved in toluene, and recooling, filtering, washing and drying are performed to obtain the white crystal 9,9-fluorene diethanol after heating and dissolution. The production cost of the 9,9-fluorene diethanol is reduced by changing the reaction conditions.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a kind of 9,9-fluorene diethanol, specifically a kind of preparation method of 9,9-fluorene diethanol. Background technique [0002] 9,9-fluorenediethanol is a kind of chemical raw material. In the prior art, more expensive reagents butyllithium and tetrahydrofuran are used to prepare, but butyllithium and tetrahydrofuran are relatively expensive substances, and the cost in the preparation process is relatively high. Moreover, the process is complicated and the yield is low. Contents of the invention [0003] Aiming at the above-mentioned technical problems in the prior art, the present invention provides a kind of preparation method of 9,9-fluorene diethanol, the preparation method of described this 9,9-fluorene diethanol solves the preparation method in the prior art The technical problems of high method cost, complex process and low yield. [0004] The invention provides a k...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/36C07C33/36C07C29/76C07C29/86C07C29/78
CPCC07C29/36C07C29/76C07C29/78C07C29/86C07C33/36
Inventor 傅志伟贺宝元潘新刚牟立娟余文卿
Owner XUZHOU B&C CHEM CO LTD
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