Immobilized fluorine-containing alcohol, method for preparing same and application of immobilized fluorine-containing alcohol
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A technology of fluorine-containing alcohols and perfluorocarbons, applied in chemical instruments and methods, catalytic reactions, organic compounds/hydrides/coordination complex catalysts, etc., can solve problems such as unsuitable for industrial production, large consumption, and troublesome recycling. Achieve the effect of novel structure, simple processing and easy preparation
Inactive Publication Date: 2016-06-15
SHIJIAZHUANG UNIVERSITY
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However, the use of expensive fluoroalcohol as a solvent requires a large amount of use and troublesome recovery, and is not suitable for large-scale industrial production.
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[0022] The structure of the catalyst (1) is shown in the following formula.
[0023]
[0024] Synthesis of styrene-divinylbenzene crosslinking resin (2% divinylbenzene) immobilized sulfonyl chloride (formula II), prepared by reference method (J.Org.Chem.1979,44,4634) (Cl content is 4.73 mmol / g).
[0025] Add 0.42g (1mmolCl) of styrene-divinylbenzene crosslinking resin immobilized sulfonyl chloride to 1.88g (8mmol) of 2,2,3,3-tetrafluoro-4-trimethylsiloxy-1-butanol, 0.28 mL (2 mmol) Et 3 N with 30mLCH 2 Cl 2 In the mixture, react at room temperature for 24h, filter, methanol (15mL×2), H 2 O (15mL×2) and methanol (15mL×2) were washed and dried in vacuo to obtain 0.88g of 2,2,3,3-tetrafluoro-4-trimethylsilyloxy-1-butanolsulfonate on immobilized basis. Through the analysis of sulfur element content, the measured sulfur content is 7.392%, and its equivalent fl...
[0029] The structure of the catalyst (2) is shown in the following formula.
[0030]
[0031] Replace 1.88g (8mmol) in Example 1 with 2.28g (8mmol) 2,2,3,3,4,4-hexafluoro-5-trimethylsiloxy-1-pentanol and 0.16g (2mmol) pyridine respectively 2,2,3,3-Tetrafluoro-4-trimethylsiloxy-1-butanol and 0.28 mL (2 mmol) Et 3 N, the other operations were the same, and 0.80 g of catalyst (2) was obtained, and the immobilized amount of fluoroalcohol was 2.29 mmol / g.
[0034] The structure of the catalyst (3) is shown in the following formula.
[0035]
[0036] Replace the 2.28g (8mmol) 2,2,3,3,4,4-hexa Fluoro-5-trimethylsilyloxy-1-pentanol was operated in the same manner to obtain 0.62 g of catalyst (3), and the immobilized amount of fluoroalcohol was 2.15 mmol / g.
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Abstract
The invention discloses an immobilized fluorine-containing alcohol catalyst (shown as a formula I), a method for preparing the immobilized fluorine-containing alcohol catalyst and application thereof.An A in the formula I is independently selected from C2-C8 saturated multi-fluorine or total-fluorine carbon chains and C2-C8 unsaturated multi-fluorine or total-fluorine carbon chains.The method for preparing the immobilized fluorine-containing alcohol catalyst shown as the formula I includes steps of a, carrying out reaction on styrene-divinylbenzene cross-linked resin and sulfonyl chloride to obtain immobilized sulfonyl chloride (shown as a formula II); b, carrying out reaction on the immobilized sulfonyl chloride (shown as the formula II) and trimethyl silica fluorine-containing alcohol (shown as a formula III) to obtain sulfonate (shown as a formula IV) with immobilized trimethyl silica fluorine-containing alcohol; c, carrying out desilylation on the sulfonate (shown as the formula IV) with the immobilized trimethyl silica fluorine-containing alcohol under the effect of tetrabutylammonium fluoride to obtain the immobilized fluorine-containing alcohol catalyst (shown as the formula I).The immobilized fluorine-containing alcohol catalyst, the method and the application have the advantages that the immobilized fluorine-containing alcohol catalyst is easy to prepare and can be recycled; the immobilized fluorine-containing alcohol catalyst can be applied to Baeyer-Villiger oxidation reaction, and products are high in yield.
Description
technical field [0001] The invention relates to the field of organic synthesis, in particular to a solid-carried fluorine-containing alcohol, a preparation method and application thereof. Background technique [0002] Fluorine-containing alcohol compounds are widely used in medicine, pesticides, fluorine-containing surfactants, dyes and other fields. Baeyer-Villiger oxidation is one of the most widely used reactions. In 1986, using the special properties of fluoroalcohols, Matsumoto et al. used 2,2,2-trifluoroethanol as solvent, cyclobutanone and 30% H without any catalyst. 2 o 2 γ-butyrolactone was prepared in high yield by Baeyer-Villiger oxidation (Heterocycles, 1986, 24, 1443). In 2000, Neumann et al. used 1,1,1,3,3,3-hexafluoro-2-propanol as solvent, ketone and 60% H 2 o 2 reaction, the corresponding lactone was also prepared in higher yield (Org.Lett.2000, 2, 2861). Both of these methods use fluorine-containing alcohols to activate H 2 o 2 The nature of the imp...
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