Ammonia → Ammonium bis(2-ethylhexyl)phosphate
Reaction equation
[P:1]([O-:21])([O:12][CH2:13][CH:14]([CH2:19][CH3:20])[CH2:15][CH2:16][CH2:17][CH3:18])([O:3][CH2:4][CH:5]([CH2:10][CH3:11])[CH2:6][CH2:7][CH2:8][CH3:9])=[O:2].[NH3:22]>CCCCCC>[P:1]([O-:21])([O:3][CH2:4][CH:5]([CH2:10][CH3:11])[CH2:6][CH2:7][CH2:8][CH3:9])([O:12][CH2:13][CH:14]([CH2:19][CH3:20])[CH2:15][CH2:16][CH2:17][CH3:18])=[O:2].[NH4+:22]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 50 °C
Procedure
To a four neck flask of 200 ml are added 19.94 g (60 mmol) of di(2-ethylhexyl) phosphate [Starting Material A] and 40.0 g of hexane at 20° C., which are gradually heated to 50° C. and thereafter 3.46 g (60 mmol) of a 29.6% aqueous solution of ammonia is added dropwise to obtain a solution of ammonium di(2-ethylhexyl) phosphate. Then, 11.8 g (20 mmol) of a 55.04% aqueous solution of lanthanum nitrate is added to this solution at a dropping rate of 1 ml/min and further the reaction is continued at the same temperature for 60 minutes. The reaction solution is left at rest to remove the separated water layer and the resulting organic phase is washed with 25 ml of water three times, and then a reflux dehydrator is mounted onto the vessel to remove water and the solvent in the reaction solution through azeotropy, and subsequently the same procedure as in [Example 1] is conducted to obtain 55.2 g of a solution of lanthanum di(2-ethylhexyl) phosphate in cyclohexane having a concentration of about 40%. The analytical results are shown in Table 1.
Sources & evidence
- ORD record
- ord-ffac6b8206244f54b9ff7935003b1c56
- Source dataset
- uspto-grants-2011_03
- Patent number
- US07906631B2
Reaction notes
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