Ammonia → HCID 131727633, compound

Participants

Reaction Steps

A 100-ml PFA-made vessel equipped with a gas inlet pipe was charged with 39.6 g of the CF3CF2CF2OCH2CF2COOH prepared in Synthesis Example 1, and nitrogen was passed through the vessel at a flow rate of 20 ml/minute for 10 minutes to deprive the system of oxygen and moisture. Fluorine gas diluted to 24% with nitrogen was passed through the vessel warmed on a water bath at 60° C. at a flow rate of 40 ml/minute for 15.3 hours. After substitution of the vessel inside atmosphere with nitrogen, 37.5 g of the reaction product was recovered. This reaction product was rectified at ordinary pressure to give 25.1 g of fraction 1 (boiling point 58° C.) and 11.9 g of fraction 2 (boiling point 80.5° C.). Gas chromatography revealed that the fraction 1 had a purity of 95% and the fraction 2 had a purity of 99.5%. Based on the results of F-NMR, the fraction 1 was identified as CF3CF2CF2OCF2CF2COOH in view of the appearance of a spectral peak at −123.3 ppm and the fraction 2 as CF3CF2CF2OCHFCF2COOH in view of the appearance of a spectral peak at −148.4 ppm. A 1-g portion of each fraction was dissolved in 10 g of water, the solution was adjusted to pH 8 by addition of aqueous ammonia, followed by drying at 80° C. under vacuum. Thus were obtained CF3CF2CF2OCF2CF2COONH4 and CF3CF2CF2OCHFCF2COONH4, respectively.

Provenance & Evidence