Phosphorus oxide (P4O10) → Perfluorooctanenitrile

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

Monoamidines were synthesized in accordance with the method of the invention as follows. In a four-neck flask, provided with a mixer, thermometer, back-flow condenser and a dropping funnel, 41.1 g (0.01 mole) of dry C7F15COOH were added and blended with 32.0 g methanol and 19. ml of concentrated H2SO4. The mixture was boiled for 6 hours, then washed with water and dried with MgSO4. The product, an ester, was distilled (Tboiling of 158° C.). The yield was 90-95% (39.2 g) using the procedure as described in U.S. Pat. No. 2,570,116 (1951). In a four-neck flask, provided with mixer, thermometer, condenser and the tube for introduction of gas, 39.2 g of C7F15COOCH3 and 100 ml diethyl ether were added. Additionally, ammonia gas was provided, and ice was used as necessary to cool the flask. The completion of the reaction was checked by gas-liquid chromatography by noting the absence of C7F15COOCH3 in the ether solution. The ether was distilled off, and the solid product was dried in air. 37.0 g of C7F15CONH2 were obtained (a yield of 97.9%) and the product had a Tboiling of 90° C. In a round-bottom flask, 37.0 g of C7F15CONH2 (0.0896 mol) that had been ground into a fine powder and 63.6 g of P2O5 were added. The materials were thoroughly mixed, and a reflux condenser was placed on the flask and heated at 100-200° C. The product C7F15—CN was obtained in an amount of 30.1 g (a yield of 85%), and had a Tboiling of 90° C. The reaction scheme as noted above appears representatively below:

Herkunft & Nachweise