A new synthetic route of Perfluoro(2-methyl-3-oxahexanoyl) fluoride

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride, A new synthetic method of this compound is introduced below., 2062-98-8

EXAMPLE 11 EXAMPLE OF PRODUCTION OF COMPOUND (71a); Into a flask (internal capacity: 300 mL) under a nitrogen gas atmosphere, CH3COCH2OH (50.0 g), R-225 (81.6 g) and NaF (85.3 g) were put, and stirring was continued while the internal temperature of the flask was kept to be at most 10C. FCOCF(CF3)OCF2CF2CF3 (213.3 g) was dropwise added thereto over a period of two hours, and then the internal temperature of the flask was returned to 25C and stirring was carried out for 12 hours. Into a filtrate obtained by pressure filtration of a solution in the flask, a saturated sodium hydrogen carbonate aqueous solution (200 mL) was added to obtain a double layered solution. The organic layer was separated and washed with water (200 mL) and dehydrated with magnesium sulfate and then concentrated by an evaporator, to obtain a concentrate (230.7 g). In the concentrate, the following compound (71a) was contained, and a GC purity of the compound (71a) was 87.2%. The reaction was separately carried out under the same conditions, whereby a concentrate (96.0 g) having a GC purity of 96.5% was obtained. The concentrate obtained by the reaction twice was distilled under reduced pressure, and as a result, a fraction (281.3 g) of 67 to 71C/1.06 kPa (absolute pressure) was obtained. The fraction was analyzed by GC and NMR, and as a result, it was confirmed that the compound (71a) having a purity of 97.9% was formed. 1H-NMR (300.4 MHz, solvent: CDCl3, standard: TMS) delta (ppm): 2.21 (s, 3H), 4.91 (q, 16.5 Hz, 2H). 19F-NMR (282.6 MHz, solvent: CDCl3, standard: CFCl3) delta (ppm): -79.6 to -80.3 (1F), -81.7 to -81.8 (3F), -82.4 to -82.5 (3F), -86.5 to -87.0 (1F), -130.1 to -130.2 (2F), -132.8 (1F).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; ASAHI GLASS COMPANY LTD.; EP1679311; (2006); A1;,
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