Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Diethyl Carbonate | HCID 7766 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | N-Propyl-Methyl Piperidinium Bis(trifluoroMethylsulfonyl)Imide | HCID 4176748 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 11512533 | HCID 11512533 | 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. 320.3 g (1.14 mol) of trifluoromethanesulfonimide was then added dropwise under strong stirring, and 264.3 g (2.2 mol) of diethyl carbonate was also added after 1 hour of reaction. The reaction mixture was transferred to an autoclave, wherein air was removed prior to heating. After 2 hours of reaction at temperature of 180° 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. 599.5 g of ethyl triphenyl phosphonium bis(trifluoromethyl sulfonyl) amide was obtained after washing 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-e56e90f426a949ccb837b1e1415e179e |
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| Source note | uspto-grants-2016_06 |
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