Tributylphosphine → HCID 87546896, compound
Reaction equation
[F:1][C:2]([P:8]([C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15])(=[O:12])[O:9]CC)([F:7])[C:3]([F:6])([F:5])[F:4].[CH2:20]([P:24]([CH2:29][CH2:30][CH2:31][CH3:32])[CH2:25][CH2:26][CH2:27][CH3:28])[CH2:21][CH2:22][CH3:23]>CCCCCC>[F:7][C:2]([P:8]([C:13]([F:18])([F:19])[C:14]([F:17])([F:16])[F:15])(=[O:9])[O-:12])([F:1])[C:3]([F:6])([F:5])[F:4].[CH2:29]([P+:24]([CH2:20][CH2:21][CH2:22][CH3:23])([CH2:25][CH2:26][CH2:27][CH3:28])[CH2:2][CH3:3])[CH2:30][CH2:31][CH3:32]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
Ethyl bis(pentafluoroethyl)phosphinate (1.538 g; 4.7 mmol) is added to cooled (0° C.) tributylphosphine (0.953 g; 4.7 mmol) in a 25 ml glass flask. The reaction mixture is stirred at 0° C. for 1 h, with initially a two-phase system and later the formation of a solid being observed. The reaction mixture is diluted with 10 ml of n-hexane, warmed and stirred at room temperature for 5.5 h. The readily volatile constituents are removed in vacuo (10−3 mbar) at 35° C. Tributylethylphosphonium bis(pentafluoroethyl)phosphinate, [(C4H9)3PC2H5][(C2F5)2P(O)O], (2.262 g; 4.2 mmol) is isolated as colourless solid in a yield of 89% and a purity of 98%.
Workup
- temperaturewarmed
- stirringstirred at room temperature for 5.5 h
- customThe readily volatile constituents are removed in vacuo (10−3 mbar) at 35° C
Sources & evidence
- ORD record
- ord-6362163ad6af4e5b92424e365f63d2d0
- Source dataset
- uspto-grants-2015_06
- Patent number
- US09056881B2
Reaction notes
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