Reaction equation
[OH-].[La+3:2].[OH-].[OH-].[P:5]([O-:25])([O:16][CH2:17][CH:18]([CH2:23][CH3:24])[CH2:19][CH2:20][CH2:21][CH3:22])([O:7][CH2:8][CH:9]([CH2:14][CH3:15])[CH2:10][CH2:11][CH2:12][CH3:13])=[O:6]>Br.C1CCCCC1>[P:5]([O-:25])([O:7][CH2:8][CH:9]([CH2:14][CH3:15])[CH2:10][CH2:11][CH2:12][CH3:13])([O:16][CH2:17][CH:18]([CH2:23][CH3:24])[CH2:19][CH2:20][CH2:21][CH3:22])=[O:6].[La+3:2].[CH2:14]([CH:9]([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:8][O:7][P:5]([O-:25])([O:16][CH2:17][CH:18]([CH2:23][CH3:24])[CH2:19][CH2:20][CH2:21][CH3:22])=[O:6])[CH3:15].[CH2:14]([CH:9]([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:8][O:7][P:5]([O-:25])([O:16][CH2:17][CH:18]([CH2:23][CH3:24])[CH2:19][CH2:20][CH2:21][CH3:22])=[O:6])[CH3:15]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Conditions
- Temperature
- 35 °C
Procedure
To a four neck flask of 200 ml are added 3.80 g (20 mmol) of lanthanum hydroxide, 19.94 g (60 mmol) of di(2-ethylhexyl) phosphate [Starting Material A] and 150 g of cyclohexane at 20° C., and then 675 mg (2.6 mmol) of 35% hydrobromic acid is added and agitated, whereby reaction is immediately started and a temperature of a reaction solution is raised up to 35° C. As the reaction solution becomes translucent while the reaction is continued at this temperature, the temperature of the reaction solution is raised to 70° C. by gradually heating. Further, the reaction is continued at this temperature, and the reaction is completed at a time point that turbidity disappears and the reaction solution becomes transparent. The reaction time is 120 minutes. Then, the same procedure as in [Example 1] is conducted to obtain 110.2 g of lanthanum di(2-ethylhexyl) phosphate having a concentration of about 20%. The analytical results are shown in Table 1.
Workup
- customwhereby reaction
- temperaturethe temperature of the reaction solution is raised to 70° C.
- temperatureby gradually heating
Sources & evidence
- ORD record
- ord-5e2b4a5a45a14339a7658b2008d9b4d9
- Source dataset
- uspto-grants-2011_03
- Patent number
- US07906631B2
Linked notes
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