JP2018048086A5 - - Google Patents

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JP2018048086A5
JP2018048086A5 JP2016183751A JP2016183751A JP2018048086A5 JP 2018048086 A5 JP2018048086 A5 JP 2018048086A5 JP 2016183751 A JP2016183751 A JP 2016183751A JP 2016183751 A JP2016183751 A JP 2016183751A JP 2018048086 A5 JP2018048086 A5 JP 2018048086A5
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alcohol compound
crystal
alcohol
represented
weight
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JP2016183751A
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Japanese (ja)
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JP2018048086A (en
JP6931984B2 (en
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Claims (6)

以下(i)及び(ii)に示す特徴を有する、以下式(1)で表されるアルコール化合物の結晶。
(i)示差走査熱量分析により得られる吸熱ピークを148〜151℃の範囲に有し、更に165〜200℃の範囲に少なくとも一つの吸熱ピークを有する。
(ii)赤外スペクトルにおいて1153±2(cm −1 )のピークを実質的に有さない
Figure 2018048086
The crystal of the alcohol compound represented by the following formula (1) which has the characteristics shown below (i) and (ii) .
(I) It has an endothermic peak obtained by differential scanning calorimetry in the range of 148 to 151 ° C., and further has at least one endothermic peak in the range of 165 to 200 ° C.
(Ii) substantially no peak at 1153 ± 2 (cm −1 ) in the infrared spectrum .
Figure 2018048086
以下(i)及び(ii)に示す特徴を有する、以下式(1)で表されるアルコール化合物の結晶。The crystal of the alcohol compound represented by the following formula (1) which has the characteristics shown below (i) and (ii).
(i)示差走査熱量分析により得られる吸熱ピークを148〜151℃の範囲に有し、更に165〜200℃の範囲に少なくとも一つの吸熱ピークを有する。(I) It has an endothermic peak obtained by differential scanning calorimetry in the range of 148 to 151 ° C., and further has at least one endothermic peak in the range of 165 to 200 ° C.
(ii)以下式(1)で表されるアルコールを95重量%以上含み、かつ芳香族炭化水素類の含量が1重量%以下である。(Ii) 95 weight% or more of alcohol represented by following formula (1) is contained, and the content of aromatic hydrocarbons is 1 weight% or less.
Figure 2018048086
Figure 2018048086
上記式(1)で表されるアルコールを95重量%以上含み、かつ芳香族炭化水素類の含量が1重量%以下である、請求項1記載のアルコール化合物の結晶。 Include alcohol represented by the formula (1) 95 wt% or more, and the content of aromatic hydrocarbons is below 1% by weight, of claim 1 Symbol placement alcohol compound crystal. 嵩密度が0.3〜0.6g/cmである、請求項1〜3いずれか1項記載のアルコール化合物の結晶。 The crystal of the alcohol compound according to any one of claims 1 to 3 , which has a bulk density of 0.3 to 0.6 g / cm3. 上記式(1)で表されるアルコール12gを、純度99重量%以上のN,N−ジメチルホルムアミド30mLに溶解させた溶液の黄色度(YI値)が10以下となる、請求項1〜4いずれか1項記載のアルコール化合物の結晶。   The yellowness (YI value) of a solution obtained by dissolving 12 g of an alcohol represented by the above formula (1) in 30 mL of N, N-dimethylformamide having a purity of 99% by weight or more is 10 or less. Or crystals of the alcohol compound according to item 1. 以下、(i)、(ii)及び(iii)の工程をこの順で含む、請求項1〜5いずれか一項記載のアルコール化合物の結晶の製造方法。
(i)
上記式(1)で表されるアルコール化合物、芳香族炭化水素類及びメタノールを含む溶液を調製する工程。
(ii)
前記溶液から25℃以上で前記アルコール化合物の結晶を析出させ、析出した結晶を分離取得する工程。
(iii)
前記結晶を100℃以上とする工程。
The manufacturing method of the crystal | crystallization of the alcohol compound as described in any one of Claims 1-5 which includes the process of (i), (ii), and (iii) in this order in the following.
(I)
A step of preparing a solution containing the alcohol compound represented by the above formula (1), an aromatic hydrocarbon and methanol.
(Ii)
A step of precipitating crystals of the alcohol compound from the solution at 25 ° C. or higher, and separating and obtaining the precipitated crystals.
(Iii)
Making the crystal at 100 ° C. or higher.
JP2016183751A 2016-09-21 2016-09-21 Crystals of alcohol compounds having a fluorene skeleton and methods for producing them Active JP6931984B2 (en)

Priority Applications (1)

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Related Child Applications (1)

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JP2019077728A Division JP2019108408A (en) 2019-04-16 2019-04-16 Crystal of alcohol compound having fluorene skeleton and method for producing the same

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JP2018048086A JP2018048086A (en) 2018-03-29
JP2018048086A5 true JP2018048086A5 (en) 2019-05-30
JP6931984B2 JP6931984B2 (en) 2021-09-08

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20210025010A (en) * 2018-06-27 2021-03-08 혼슈우 카가쿠고교 가부시키가이샤 Crystalline of 9,9-bis(4-hydroxyphenyl)-2,3-benzofluorene
JP7379770B2 (en) * 2018-09-19 2023-11-15 本州化学工業株式会社 Crystalline form of bisfluorene compound
WO2020059709A1 (en) * 2018-09-19 2020-03-26 本州化学工業株式会社 Crystal mixture of bisfluorene compound

Family Cites Families (6)

* Cited by examiner, † Cited by third party
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JP3521242B2 (en) * 1997-03-05 2004-04-19 大阪瓦斯株式会社 Purification method of biscresols
JP2001206863A (en) * 2000-01-25 2001-07-31 Osaka Gas Co Ltd Fluorene compound and method for the same
CN101657406B (en) * 2007-02-15 2014-04-02 田冈化学工业株式会社 Crystalline polymorph of fluorene derivative and process for production thereof
JP5325627B2 (en) * 2008-03-27 2013-10-23 大阪瓦斯株式会社 Method for producing alcohol having fluorene skeleton
WO2013133106A1 (en) * 2012-03-09 2013-09-12 本州化学工業株式会社 Method for producing 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, crystal of said compound, and method for producing said crystal
JP6210555B2 (en) * 2014-04-03 2017-10-11 田岡化学工業株式会社 Method for recovering bisphenolfluorenes from a polyester resin having a fluorene structure

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