trifluoro(1,1,2,2-tetrafluoro-2-iodoethoxy)ethylene synthesis

Yield:6037-91-8 99.9%

Reaction Conditions:

with sodium iodide in dimethyl sulfoxide at 23 - 85; for 1.5 h;Product distribution / selectivity;

Steps:

1

EXAMPLE 1; In a 100 ml three-neck flask equipped with a Dimroth condenser and a dropping funnel were placed 30 g of DMSO and 30.4 g (202.4 mmol) of NaI. Through the dropping funnel was added dropwise 20.0 g (67.5 mmol) of CF₂CFOCF₂CF₂SO₂Cl, with stirring at room temperature (23.0° C.). During the dropwise addition, the solution was heated by self-heating to a maximum of 85° C., and changed its color from colorless to reddish brown. After the completion of dropwise addition, the solution was further reacted with stirring for 1.5 hours. After the completion of reaction, the solution was separated into two phases by addition of water and CCl₄, and the organic CCl₄ phase was analyzed by gas chromatography and ¹⁹F-NMR. As a result, the formation of the target compound CF₂CFOCF₂CF₂I was confirmed. The CF₂CFOCF₂CF₂SO₂Cl conversion ratio was 100.0%; CF₂CFOCF₂CF₂I selectivity was 99% or more; and CF₂CFOCF₂CF₂I yield was 99.9% or more.

References:

US2007/185355,2007,A1 Location in patent:Page/Page column 8