Fluorination reagent and deoxygenation fluorination method
A fluorinated reagent and fluorinated technology, applied in chemical instruments and methods, organic chemistry, steroidal compounds, etc., can solve the problems of poor stability and high cost, and achieve the effect of high tolerance
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[0037] The fluorinated reagent can be prepared by existing preparation methods:
[0038] For example, in some embodiments, the perfluoropolyether chain carboxylate provided by the present invention can be prepared by reacting a perfluoropolyether chain carboxylate with a base.
[0039] Another embodiment of the present invention provides a method for deoxyfluorination, comprising the following steps:
[0040] adding a fluorinating reagent as described above to an alcoholic substrate;
[0041] The deoxyfluorination reaction is carried out to obtain fluorine-containing products.
[0042] In some embodiments, fluoride salts are also added in the deoxyfluorination reaction.
[0043] The inventors have found through a large number of experiments that the addition of fluorine salts in the deoxyfluorination reaction in which the fluorinating reagent participates can effectively increase the yield of fluorine-containing products, and the addition of fluorine salts has a greater impa...
Embodiment 1
[0062] In this example, CF 3 OCF 2 OCF 2 CO 2 K is an example to illustrate the preparation method of perfluoropolyether chain carboxylate provided by the present invention, comprising the following operations:
[0063] Add CF to a 500mL single-necked bottle 3 OCF 2 OCF 2 CO 2 C 2 h 3(54.8g, 0.2mol) and 150mL of ethanol, and KOH (10.1g, 0.18mol) was dissolved in 10mL of water, and the KOH aqueous solution was added dropwise into the single-necked bottle with a syringe, and stirred vigorously after the addition, and reacted overnight at room temperature . After the reaction was completed, the solvent was removed under reduced pressure, and the water was removed overnight with an oil pump under the condition of heating at 50°C to obtain 55.7g of white solid CF 3 OCF 2 OCF 2 CO 2 K.
[0064] Concrete reaction formula is as follows:
[0065]
Embodiment 2
[0067] This embodiment is used to illustrate the deoxyfluorination method disclosed in the present invention, comprising the following steps:
[0068] Weigh 4-phenylbutanol (0.2mmol, 1.0equiv) and CF in a 10mL dried Shrek tube 3 OCF 2 OCF 2 CO 2 K (0.1mmol, 0.5equiv), weighed CsF (0.1mmol, 0.5equiv) in the glove box, and added 1mL solvent DMPU (N,N-dimethylpropenyl urea), and reacted at 150°C under nitrogen atmosphere for 5 Hour. After the reaction was completed, cool to room temperature and filter, add 15 mL of water to the filtrate, and add 15 mL of ethyl acetate (or dichloromethane) to extract three times, separate layers, collect the organic phase, combine the organic phase, wash once with saturated brine, anhydrous Na 2 SO 4 Dry, concentrate, and purify by silica gel column chromatography to obtain the final product.
[0069] Concrete reaction formula is as follows:
[0070]
PUM
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