Water → HCID 131724699, compound

Temperature

65 °C

In a procedure similar to that described in Preparation of Precursor 1, FSO2(CF2)3COF (70 g, 0.25 mole), KF (21.8 g, 0.37 mole), diglyme (350 ml), Adogen 464 (10.5 g of a 56% solution in anhydrous diglyme) and diethyl sulfate (48 g, 0.312 mole) were combined and reacted at 52° C. for 16 hours. Deionized water (˜250 g) was carefully added and the reaction mixture allowed to stir at about 65° C. for two hours. This was followed by heating the solution to about 105° C. and steam distilling the product into a Dean Stark trap after which the lower fluorochemical-containing phase was separated from the upper aqueous phase. The lower fluorochemical-containing phase mixture was distilled 51.3 g (147° C.) to yield FSO2(CF2)4OC2H5 (51.3 g); The product structure, which included three branched chain isomers, was confirmed by gc/ms, 1H and 19F NMR. FSO2(CF2)4OC2H5 (30.8 g, 0.094 mole) was treated with excess lithium hydroxide as described in Preparation 3 and converted to LiO3S(CF2)4OC2H5 (30.2 g). The product structure was confirmed by lc/ms and 1H and 19F NMR. A small impurity of CF3CFHOC4F8SO3Li was observed in the liquid chromatography/mass spectrometry (lc/ms).

1. customreacted at 52° C. for 16 hours
2. temperatureby heating the solution to about 105° C.
3. distillationsteam distilling the product into a Dean Stark trap after which the
4. additionlower fluorochemical-containing phase
5. customwas separated from the upper aqueous phase
6. additionThe lower fluorochemical-containing phase mixture
7. distillationwas distilled 51.3 g (147° C.)

ORD record

ord-1258c5a615604dbdb115b868ebea25a4

Source dataset

uspto-grants-2005_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06841333B2