- Preparation method of 2, 2-bis (4-aminophenyl) hexafluoropropane
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The invention belongs to the technical field of compounds, and particularly relates to a preparation method of 2, 2-bis (4-aminophenyl) hexafluoropropane. The invention relates to a preparation method of 2, 2-bis-- (4-aminophenyl) hexafluoropropane, which is characterized by comprising the following steps: S1, reacting a compound I with an amine compound in the presence of a catalyst to obtain a compound II; and S2, treating the compound II to obtain the 2, 2-bis (4-aminophenyl) hexafluoropropane. The preparation method provided by the invention mainly solves the problems of high risk, high product separation and purification difficulty, harsh reaction conditions and the like in the traditional synthesis method. According to the method, 2, 2-bis (4-halogen phenyl) hexafluoropropane or 2, 2-bis (4-trifluoromethanesulfonyl phenyl) hexafluoropropane is used as a raw material, the raw material and an amine compound are subjected to a substitution reaction under the condition of a catalyst, and then a target product is obtained through deprotection and purification. The method has the advantages of mild reaction conditions, easiness in product purification, high reaction yield and the like.
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Paragraph 0068-0070; 0072
(2021/04/10)
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- Green preparation method of 2,2-bis(4-aminophenyl)hexafluoropropane
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The invention relates to the field of fine organic synthesis, in particular to a green preparation method of 2,2-bis(4-aminophenyl)hexafluoropropane. The green preparation method comprises the following steps: (a) carrying out oxidation reaction on 2,2-bis(4-methylphenyl)hexafluoropropane and oxygen in a perfluorinated compound solvent, and conducting separating to obtain 2,2-bis (4-carboxyphenyl)hexafluoropropane; (b) carrying out a reflux reaction on the compound obtained in the step (a) and ammonia gas in an organic solvent to obtain ammonium salt of 2,2-bis(4-carboxylphenyl)hexafluoropropane; (c) mixing the compound obtained in the step (b) with an organic solvent, carrying out heating, and raising a temperature for dehydrating to obtain 2,2-bis(4-formamidophenyl)hexafluoropropane; and (d) carrying out a Hofmann degradation reaction on the compound obtained in the step (c) and sodium hypochlorite in a hydrofluoroether solvent, and carrying out purifying to obtain the 2,2-bis(4-aminophenyl)hexafluoropropane. According to the invention, a selected oxidizing agent is economical and green, and the oxidizing solvent is non-combustible and non-explosive; and a hydrofluoroether solvent is selected for the Hofmann reaction, so high-COD wastewater is reduced, and industrial production is facilitated.
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- Synthesis method of 2,2-bis(4-aminophenyl)hexafluoropropane
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The invention relates to a 2,2-bis(4-aminophenyl)hexafluoropropane synthesis method, which comprises: adopting a compound represented by a formula I as a raw material, adopting nickel chloride as a catalyst, adopting guanidine hydrochloride as an ammonia source, and carrying out a reaction to obtain a compound represented by a formula II, wherein the compound represented by the formula II is the target product 2,2-bis(4-aminophenyl)hexafluoropropane. According to the invention, a brand-new reaction route is provided, bisphenol AF which is cheap and easy to obtain is adopted as a raw material,nickel chloride is adopted as a catalyst, guanidine hydrochloride is adopted as an ammonia source, and the reaction step is shortened into one step in a high-pressure kettle, so that operation is easy, safety is high, the yield is high, and industrial production is easy to achieve.
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Paragraph 0008; 0021-0033
(2020/07/12)
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- Novel synthetic method for 2,2-bis(4-aminophenyl)hexafluoropropane
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The invention relates to a novel synthetic method for 2,2-bis(4-aminophenyl)hexafluoropropane. The novel synthetic method is mainly to solve problems like high hazards, large product separation and purification difficulties, expensive raw materials and harsh reaction conditions in a traditional synthetic method. The method comprises the following steps: with 2,2-bis(4-methylphenyl)hexafluoropropane as a raw material, oxidizing the 2,2-bis(4-methylphenyl)hexafluoropropane into 2,2-bis(4-carboxylphenyl)hexafluoropropane through chromium trioxide, then carrying out an acyl chlorination reaction,introducing ammonia gas, carrying out an amidation reaction so as to obtain 2,2-bis(4-formamidophenyl)hexafluoropropane, and carrying out a Hoffman reaction in a sodium hypochlorite solution so as toobtain a target product. The method provided by the invention has the advantages of cheap and easily-available raw materials, mild reaction conditions, easy industrialization, etc.
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- Functionalized Photoreactive Compounds
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The present invention concerns functionalized photoreactive compounds of formula (I), that are particularly useful in materials for the alignment of liquid crystals. Due to the adjunction of an electron withdrawing group to specific molecular systems bearing an unsaturation directly attached to two unsaturated ring systems, exceptionally high photosensitivities, excellent alignment properties as well as good mechanical robustness could be achieved in materials comprising said functionalized photoreactive compounds of the invention.
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- Process of preparing 2,2-bis(4-aminophenyl)-hexafluoropropane
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2,2-Bis(4-aminophenyl)hexafluoropropane is prepared by the steps of (a) reacting 2,2-bis(4-carboxyphenyl)hexafluoropropane with thionyl chloride at 80°-150° C. in a water insoluble organic liquid in the presence of a catalyst such as dimethylformamide to obtain a solution of 2,2-bis(4-chloroformylphenyl)hexafluoropropane, (b) mixing the obtained solution with an aqueous solution of sodium azide to obtain an acid azide solution, (c) heating the organic phase of the acid azide solution to 80° C. or above to cause rearrangement of the acid azide into an isocyanate, (d) hydrolyzing the isocyanate by mixing the isocyanate solution with an acid such as 40-80% sulfuric acid to form a salt of the aimed diamine as an aqueous solution mixed with an organic phase, and (e) neutralyzing the aqueous solution separated from the liquid mixture obtained at step (d) to precipitate the aimed diamine. This process is favorable for industrial practice because the main steps (a) to (d) are all reactions in organic liquids without precipitating solid intermediates.
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