Synthetic method of perfluorovinyl perfluoroiodoethyl ether and its intermediate
A synthetic method and iodine technology, which is applied in chemical instruments and methods, preparation of organic compounds, carboxylate preparation, etc., can solve the problems of long and cumbersome routes and high risk factors, and achieve short routes, small risk factors and easy operation easy effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0047] The synthesis of embodiment 1 compound 2
[0048]
[0049] Add hydrosulfite (60.9g, 350mmol), sodium bicarbonate (58.8g, 700mmol), deionized water (175mL), acetonitrile (175mL) into the three-necked flask equipped with a reflux condenser, stir to make the solid dissolve completely, slowly Compound 1 (60.0 g, 175 mmol) was added, and after the addition was completed, the reaction was carried out at 95° C. in an oil bath for 4 h. Filter the solid, remove water and acetonitrile from the liquid phase under reduced pressure (water bath temperature 46°C) to obtain a white solid, dissolve the solid with hot acetonitrile (100mLx3), filter off the insoluble matter, and dry the organic phase with anhydrous sodium sulfate. After filtration, the solvent was removed to give compound 2 (62 g, 97%).
Embodiment 2
[0050] The synthesis of embodiment 2 compound 3
[0051]
[0052] At room temperature, sodium persulfate (118g, 498mmol), elemental iodine (126g, 498mmol), water (220mL), and acetonitrile (220mL) were added to a three-necked flask, and compound 2 (55g, 149mmol) in acetonitrile ( 100mL)-water (100mL) solution, after addition, react overnight. A small amount of sodium sulfate is added to the reaction system, and stratification occurs. The upper black solution is quenched with saturated sodium sulfite until the system is light yellow, sodium sulfate (50g) is added, and the liquid is separated. The aqueous phase is extracted once with ethyl acetate, and the organic mixture is combined. phase, dried over anhydrous sodium sulfate, and filtered to remove the solvent to obtain light compound 3 (53 g, 92%).
Embodiment 3
[0053] The synthesis of embodiment 3 compound 4
[0054]
[0055] Compound 3 (30g, 77.5mmol) was dissolved in water (20mL) and methanol (20mL) and potassium hydroxide (4.34g, 77.5mmol) was slowly added under vigorous stirring. After 30 minutes of reaction, the solvent was removed under reduced pressure to obtain a light yellow solid. The solid was dried in a vacuum oven until the weight was no longer changed, and the temperature of the solid was rapidly raised to 130° C. for decarboxylation to obtain compound 4 (21.5 g, 84%).
[0056] 19 F NMR (376MHz, CDCl 3 )δppm-65.00(m,2F),-87.79(m,2F),-113.76(ddd,J=84.1,65.3,4.6Hz,1F),-121.73(ddq,J=112.0,84.1,4.8Hz,1F ), -135.04 (ddq, J=112.1, 65.2, 4.2Hz, 1F).
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More