Method of preparing a fluorene derivative and the method of purifying thereof
AssigneeOsaka Gas Co., Ltd.
InventorsMitsuaki Yamada, Katsuhide Okimi, Katsuyuki Takahashi, Norio Nagano
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AssigneeOsaka Gas Co., Ltd.
InventorsMitsuaki Yamada, Katsuhide Okimi, Katsuyuki Takahashi, Norio Nagano
Estimating the term…
A fluorene derivative of high purity is produced by reacting fluorenone with phenoxyethanol in the presence of a sulfuric acid-thiol catalyst system, dissolving the reaction mixture in a lower aliphatic alcohol and adding water to the resulting solution for precipitation of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene [fluorene derivative]. A fluorene derivative of still higher purity is obtained by recrystallization from a lower aliphatic alcohol. In accordance with this invention, a fluorene derivative can be produced advantageously on a commercial scale without incurring any appreciable loss of fluorenone, in good yield, with high efficiency and in a reduced production time.
A method of preparing a fluorene derivative which comprises reacting fluorenone with phenoxyethanol to synthesize 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene at 30.degree.-150.degree. C. using as a catalyst, per mol of fluorenone, 80-200 ml of sulfuric acid of not less than 75% concentration and 0.1-10 ml of at least one thiol compound selected from the group consisting of ethylmercaptan, n-butylmercaptan, 1-octylmercaptan, t-dodecylmercaptan, mercaptoethanol, mercaptoacetic acid and .beta.-mercaptopropionic acid.
Dependencies are inferred from the claim text.