1,3-bis(hydroxyphenyl)-5-ethyladamantane compound and method for production thereof, and aromatic polycarbonate resin and method for production thereof
A polycarbonate resin, ethyladamantane technology, applied in the field of new 1,3-bis-5-ethyladamantane compound, aromatic polycarbonate resin, can solve unknown problems and other problems
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[0108] Hereinafter, although an Example is given and this invention is demonstrated in more detail, this invention is not limited to these Examples.
[0109] [Analytical method]
[0110] (1) GC-FID analysis
[0111] A capillary column DB-1 (30 m, inner diameter 0.53 mm, film thickness 1.5 μm) manufactured by Agilent was installed in a gas chromatograph HP-6890 manufactured by Hewlett Packard, and analyzed with an FID detector.
[0112] (2) GC / MS analysis
[0113] A capillary column DB-1MS (30 m, inner diameter 0.250 mm, film thickness 0.25 μm) manufactured by Agilent was installed in a gas chromatography mass spectrometer GCMS-QP2010Ultra manufactured by Shimadzu Corporation, and analyzed.
[0114] (3) NMR analysis
[0115] The measurement sample was dissolved in acetone-D6 to prepare a 10% solution, and the measurement was performed using a JNM-AL400 nuclear magnetic resonance apparatus manufactured by JEOL Ltd.
[0116] (4) Melting point
[0117] The melting point was m...
manufacture example 1
[0123] [Manufacturing example] Synthesis of 1,3-dihydroxy-5-ethyladamantane
[0124] 1,3-Dihydroxy-5-ethyladamantane was synthesized according to the method described in Example VI of US Patent No. 3383424.
[0125] That is, 1890 g of hydrous acetic acid (moisture concentration 15%) and 609 g of chromium trioxide as a source of chromic acid were put into a detachable flask with a capacity of 5 L, and 1-ethanediol was added dropwise over 30 minutes while stirring with a mechanical stirrer. Adamantane 200g. During the dropwise addition, heat was generated, and the liquid temperature rose from room temperature up to 90°C. Thereafter, the liquid temperature was maintained at 80 to 90° C., and the reaction was continued for 3.5 hours.
[0126] After completion of the reaction, the reaction product was cooled to room temperature, and the precipitated crystals were separated with a glass filter to obtain 221 g of crude crystals of 1,3-dihydroxy-5-ethyladamantane. The obtained crud...
Embodiment 1
[0129] Synthesis of 1,3-bis(4-hydroxyphenyl)-5-ethyladamantane
[0130] 170 g (0.866 mol) of 1,3-dihydroxy-5-ethyladamantane and 652 g (6.93 mol) of phenol were added to a 2 L separable flask, and the temperature was raised to 85° C. while stirring with a mechanical stirrer. When the temperature reached 85°C, 85 g (0.867 mol) of concentrated sulfuric acid was added dropwise over 20 minutes. During the dropwise addition, heat was generated and the maximum temperature rose to 95°C. After completion of the dropwise addition, the liquid temperature was adjusted to 90° C., and the reaction was continued for 5 hours. After 5 hours, the reaction solution was poured into a container containing 2 L of ice water. Furthermore, 24% sodium hydroxide aqueous solution was added until pH became 7, and it neutralized.
[0131] 500 ml of ethyl acetate was added to the obtained reaction product, and extraction with ethyl acetate was repeated three times. The extracted ethyl acetate solution ...
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