Nitrogen → HCID 131735796, compound

HRID 2204019Notes

Reaction equation

N#N.[CH2:3]([P:5]([CH2:12][CH3:13])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH3:4].[N-:14]([S:22]([C:25]([F:28])([F:27])[F:26])(=[O:24])=[O:23])[S:15]([C:18]([F:21])([F:20])[F:19])(=[O:17])=[O:16].[C:29](=O)(OC)OC>CO>[F:28][C:25]([F:26])([F:27])[S:22]([N-:14][S:15]([C:18]([F:19])([F:20])[F:21])(=[O:16])=[O:17])(=[O:23])=[O:24].[CH2:12]([P+:5]([CH2:3][CH3:4])([CH3:29])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH3:13]

Participants

Conditions

Temperature: 15 °C

Procedure

In a reactor wherein air was replaced by N2, 200.0 g of (1.2 mol) diethylphenyl phosphine and 400 mL of methanol were added and cooled to 15° C. by a ice-bath. 338.6 g (1.2 mol) of trifluoromethanesulfonimide was then added dropwise under strong stirring, and 202.0 g (2.2 mol) of dimethyl carbonate was also added after the reaction was complete. 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 1.2 MPa to 1.5 MPa, the crude product was obtained after distilling off the unreacted materials and solvent. 507.1 g of diethyl methyl phenyl phosphonium bis(trifluoromethanesulfonyl)amide was obtained after washing and drying at 60° C. and 0.1 kPa for 4 hours.

Workup

additionwere added
additionwas also added after the reaction
customwas removed
temperatureto heating
customAfter 2 hours of reaction at temperature of 180° C.
customat pressure of from 1.2 MPa to 1.5 MPa, the crude product was obtained
distillationafter distilling off the unreacted materials and solvent

Sources & evidence

ORD record: ord-54976bf8d99049eaa27f76e57c462c30
Source dataset: uspto-grants-2016_06
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09365596B2

Reaction notes

Loading…