Process for purification of oligoanilines and oligoanilines
A technology of oligoaniline and purification method, which is applied in the fields of amino compound purification/separation, organic chemistry, organic material conductor, etc. Ensuring reproducible, easy-to-manage effects
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[0114] The following examples and comparative examples are given to describe the present invention more specifically, but the present invention is not limited to the following examples.
Synthetic example 1
[0116] Phenyltetraphenylamine (hereinafter referred to as PTA) shown in formula (6) is prepared from p-hydroxy Diphenylamine and p-phenylenediamine were synthesized (light blue solid, yield 85%).
[0117]
[0118] [1] Purification method of oligoaniline compound
Embodiment 1
[0120] In a 1L three-necked round-bottomed flask, 20 g (0.0452 mmol) of PTA obtained in Synthesis Example 1 and 2.0 g (10% by mass relative to PTA) of activated carbon (manufactured by Junsei Chemical Co., Ltd.) were added under a nitrogen atmosphere, and the 500 g of degassed dehydrated 1,4-dioxane (manufactured by Kanto Chemical Co., Ltd.).
[0121] Next, while the internal temperature was kept at 90° C. using an oil bath, it was heated and stirred for 1 hour to completely dissolve PTA. Then, use Kiriyama glass (S-60), Kiriyama filter paper (3C), and 50 g of fluoromagnesite (fluoromagnesite 545, manufactured by Junsei Chemical Co., Ltd.) as a stationary phase, and keep warm in a water circulation device with a temperature controller. Filtrate while hot at 90°C to remove activated carbon.
[0122] The filtrate was left to cool until the internal temperature reached 20°C. After cooling, the lavender solution that precipitated PTA was directly put into the reaction vessel, mo...
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