Nitrogen → Tributyl(methyl)phosphanium bis(trifluoromethanesulfonyl)azanide

Participants

Reaction Conditions

Reaction Steps

In an reactor wherein air was replaced by N2, 300.0 g (1.5 mol) of tributyl phosphine and 1000 mL of methanol were added and cooled to about 0° C. by a ice-bath. 427.6 g (1.5 mol) of trifluoromethanesulfonimide was then added dropwise under strong stirring, and 202.0 g (2.2 mol) of dimethyl carbonate was also added afterwards. After one hour of reaction and mixing, the reaction mixture was transferred to an autoclave, wherein air was removed prior to heating. After 6 hours of reaction at temperature of 180° C. and pressure of from 1.6 MPa to 1.7 MPa, the crude product was obtained after distilling off the unreacted materials and solvent. 705.7 g of methyl tributyl phosphonium bis(trifluoromethanesulfonyl)amide was obtained after washing and drying at 60° C. and 0.1 kPa for 4 hours.

Provenance & Evidence