Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Dimethyl Carbonate | HCID 12021 | — |
| Reactant | N-Propyl-Methyl Piperidinium Bis(trifluoroMethylsulfonyl)Imide | HCID 4176748 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 131735794 | HCID 131735794 | 95.4% |
Reaction Steps
In a reactor wherein air was replaced by N2, 300.0 g of (1.1 mol) triphenyl phosphine and 500 mL of methanol were added and cooled to 10° C. by a ice-bath. 321.8 g (1.1 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 4 hours of reaction at temperature of 160° C. and at pressure of from 1.4 MPa to 1.5 MPa, the crude product was obtained after distilling off the unreacted materials and solvent. 584.8 g of methyl triphenyl phosphonium bis(trifluoromethanesulfonyl)amide was obtained after recrystallization and drying at 60° C. and 0.1 kPa for 4 hours.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09365596B2 |
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| Source dataset | uspto-grants-2016_06 |
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| ORD ID | ord-72843b1adfc04db488509cbaf7979fd6 |
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| Source note | uspto-grants-2016_06 |
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