Electric Literature of 13353-03-2,Some common heterocyclic compound, 13353-03-2, name is 2,4,6,8-Tetraoxanonane, molecular formula is C5H12O4, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
To 250ml four-necked flask was added under mechanical stirring phenol (phenol and paraformaldehyde dimethyl ether molar ratio of 15:1), phosphoric acid (the molar ratio of phosphoric acid to paraformaldehyde dimethyl ether is 6.4: 1) and water (molar ratio of water and paraformaldehyde dimethyl etherRatio of 14: 1), the water bath was slowly heated to 80 C, and then 5 g of paraformaldehyde dimethyl ether was slowly added dropwise during the controlTemperature between 75 -85 C . Bi completed, maintaining the temperature at 80 C to continue the reaction 4h. Complete the reaction of raw materials, natural cooling to 45 C ,The reaction solution was poured into a separatory funnel, standing stratification, the lower phosphoric acid aqueous solution recovery applied. After the upper organic phase is neutralized by alkali,Concentrated under reduced pressure, the application of excess phenol recovery. The concentrate was diluted with ethyl acetate and washed successively with saturated aqueous ammonium chloride solutionWashed with water, dried over anhydrous sodium sulfate, suction filtered, the filtrate was concentrated to dry twice to obtain the crude product. Crude by high pressure liquid chromatographyMeasured, bisphenol F yield, selectivity and product distribution in Table 2.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,4,6,8-Tetraoxanonane, its application will become more common.
Reference:
Patent; Yancheng Tonghai Biological Technology Co., Ltd.; Wang Hui; Shen Jianyi; Zhao Yupei; Zhu Jian; Wang Yang; (10 pag.)CN105152866; (2017); B;,
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