Sodium Hydroxide → Bis(2-ethylhexyl) sodium 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].[OH-].[Na+:23]>>[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].[Na+:23]Participants
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 12.0 g (60 mmol) of a 20% aqueous solution of sodium hydroxide at 20° C., which are agitated for 60 minutes to obtain an aqueous solution of sodium di(2-ethylhexyl) phosphate. Then, 80 g of ethanol is added to this solution and subsequently 17.87 g (20 mmol) of a 26.0% aqueous solution of lanthanum chloride is added at a dropping rate of 1 ml/min, which are further reacted at the same temperature for 0 minute with stirring, whereby lanthanum di(2-ethylhexyl) phosphate is gradually precipitated to cause white turbidity in the solution. The precipitates are dissolved by adding 80 g of cyclohexane to the solution with stirring. The reaction solution is left at rest to remove the separated water layer. After the washing with 25 ml of water three times, a reflux dehydrator is mounted onto the vessel to remove water and ethanol in the reaction solution through azeotropy with cyclohexane, and then the same procedure as in [Example 1] is conducted to obtain 53.8 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-dfee3ab1466a45f4909149515a5daf5b
- Source dataset
- uspto-grants-2011_03
- Patent number
- US07906631B2
Reaction notes
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