Carbon Dioxide → HCID 86667933, compound

Participants

Reaction Conditions

Reaction Steps

73 mL N-methylpyrrolidone (NMP) was introduced into a 500-mL autoclave; 1.5 g (17 mmol) lithium bromide and 132 g (575 mmol) 2-pentafluoroethyl-2-trifluoromethyloxirane were charged; and the interior of the system was replaced with CO2 5 times. The reaction solution was heated to 100° C. and pressurization with CO2 at 0.8 MPa was performed until the starting epoxide had disappeared. After the reaction was finished, the reaction solution was returned to room temperature; quenching was performed with 300 mL 1 N aqueous hydrochloric acid; separation was carried out and the organic layer was dried over magnesium sulfate; and suction filtration was performed. The filtrate was subjected to rectification under reduced pressure using a 10-stage Oldershaw column to obtain 113 g (isolated yield=72%, purity=99.7%) 1-trifluoromethyl-1-pentafluoroethylethylene carbonate (=4-pentafluoroethyl-4-trifluoromethyl-1,3-dioxolan-2-one). Molecular Sieve 3A (Wako Pure Chemical Industries, Ltd.) was then introduced and the water content was reduced to 30 ppm.

Provenance & Evidence