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Method for producing alcohol compound having fluorene skeleton

A technology of alcohol compounds and manufacturing methods, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of removing mercaptans, insufficient improvement of coloring, etc., and achieve the effect of less coloring

Active Publication Date: 2018-12-21
TAOKA CHEM COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] However, even with the method described in Patent Document 4, the coloring improvement is insufficient, and since a large amount of thiols are required for the reaction, it is difficult to completely remove thiols from the product. When the compound is used to make resin, there is a problem that the sulfur component derived from mercaptans causes further coloring of the resin

Method used

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  • Method for producing alcohol compound having fluorene skeleton
  • Method for producing alcohol compound having fluorene skeleton
  • Method for producing alcohol compound having fluorene skeleton

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0104] Hereinafter, although an Example etc. are given and this invention is demonstrated concretely, this invention is not limited at all. In addition, in the example, various measurements were implemented by the following method. In addition, the production rate (survival rate) and purity of each component described in the following Examples, Comparative Examples, and Reference Examples are HPLC area percentage values ​​measured under the following conditions (excluding the solvent in the reaction solution and the included The corrected area percentage value after the peak of the organic compound), and the yield is the apparent yield when the obtained alcohol represented by the above formula (1) is an inclusion body and assumed not to be an inclusion body. In addition, the so-called "polymer" in Examples and Comparative Examples means compounds obtained by further reacting one molecule or more of ethylene carbonate on the alcohol compound represented by the above formula (1)...

Embodiment 2

[0148] Add 150g (0.298mol) of 9,9'-bis(4-hydroxy-3-phenylphenyl)fluorene, 3.4g (0.025mol) of potassium carbonate to a glass reactor equipped with a stirrer, a heating cooler, and a thermometer ), 60.1 g (0.682 mol) of ethylene carbonate, 225 g of toluene, and 150 g of diethylene glycol dimethyl ether, the temperature was raised to 115° C., and after stirring at the same temperature for 13 hours, it was confirmed by HPLC that the peak of the raw material disappeared. The formation rate of the polymer at the end of the reaction was about 0.5%.

[0149] After cooling the obtained reaction liquid to 85 degreeC, 225 g of water was added, it stirred at 80-85 degreeC for 30 minutes, and after standing still, the water layer was separated. After repeating the same operation three times, the obtained organic solvent layer was partially concentrated to obtain a solution containing the alcohol compound represented by the above formula (1), toluene, and diglyme.

[0150] To this solution...

Embodiment 3～6

[0161] The reaction and post-processing were performed similarly to Example 1, and the concentrate was obtained. The obtained concentrate was divided into 4 equal parts, and toluene and methyl alcohol were added respectively so as to reach the ratio shown in the following Table 1, and crystallization and drying operations were carried out in the same manner as in the method described in Example 1 to obtain the formula (1) represented by the above formula (1). crystals of alcohol compounds. Each analysis value of each crystal is shown in Table 1 below. In addition, the addition amount of toluene and methanol in Table 1 is the ratio (weight ratio) with respect to the alcohol compound represented by said formula (1) contained in each concentrate.

[0162] [Table 1]

[0163] [Table 1]

[0164]

[0165] *1 above area (cm -1 ) in the presence or absence of peaks.

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Abstract

Provided are a method for producing an alcohol compound represented by formula (1) wherein the method includes, in this order, a step (i) for preparing a solution including an alcohol compound represented by formula (1), aromatic hydrocarbons, and methanol, a step (ii) for precipitating crystals of the alcohol compound from the solution at 25DEG C or higher and separating and acquiring the precipitated crystals, and a step (iii) for removing the methanol from the crystals at 60DEG C or higher, and crystals of an alcohol compound represented by formula (1) wherein the crystals substantially donot have a 1153+ / -2 (cm-1) peak in the infrared absorption spectrum.

Description

technical field [0001] The present invention relates to a method for producing a novel alcohol compound having a fluorene skeleton that is suitable as a monomer for forming a resin (optical resin) that constitutes an optical member such as an optical lens or an optical film, and is excellent in processability and productivity. resin. Background technique [0002] Resin materials such as polycarbonate, polyester, polyacrylate, polyurethane, and epoxy resin, which use an alcohol compound having a fluorene skeleton as a raw material monomer, have become popular in optical lenses and optical sheets in recent years due to their excellent optical properties and heat resistance. and other new optical materials have received attention. Among them, the alcohol compound having a structure represented by the following formula (1) is due to the optical properties such as refractive index, heat resistance, water resistance, chemical resistance, electrical properties, and mechanical prop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/40C07C43/23
CPCC07C41/40C07C43/23C07C41/30C07C2603/18
Inventor 加藤弘行西田有儿佐伯崇史
Owner TAOKA CHEM COMPANY
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