Reaction equation
[P:1]([O-:39])([O:33][CH2:34][CH:35]([OH:38])[CH2:36]Cl)([O:3][C:4]([F:32])([F:31])[C:5]([F:30])([F:29])[C:6]([F:28])([F:27])[C:7]([F:26])([F:25])[C:8]([F:24])([F:23])[C:9]([F:22])([F:21])[C:10]([F:20])([F:19])[CH2:11][CH2:12][CH2:13][CH2:14][C:15]([F:18])([F:17])[F:16])=[O:2].[Na+:40].C(O)C.[OH-].[Na+]>C(O)C>[P:1]([O-:39])([O:33][CH2:34][CH:35]1[O:38][CH2:36]1)([O:3][C:4]([F:32])([F:31])[C:5]([F:30])([F:29])[C:6]([F:28])([F:27])[C:7]([F:26])([F:25])[C:8]([F:24])([F:23])[C:9]([F:22])([F:21])[C:10]([F:20])([F:19])[CH2:11][CH2:12][CH2:13][CH2:14][C:15]([F:18])([F:17])[F:16])=[O:2].[Na+:40]Participants
Conditions
- Temperature
- 70 °C
Procedure
50 g (0.073 mol) of sodium heptadecafluorododecyl 2-hydroxy-3-chloropropyl phosphate was charged into a reactor, to which 1000 ml of ethanol was added, followed by agitation and heating to 70° C. to obtain a uniform mixture. Thereafter, the reaction system was cooled down to 30° C., to which was gradually added 40.5 g (0.073 mol) of a 0.0018 mol/g sodium hydroxide ethanol solution, followed by agitation for 4 hours while keeping the temperature. The HPLC analysis revealed the disappearance of a peak of the starting material with a peak for the resultant new product appearing. The resultant NaCl precipitate was removed by filtration and the ethanol was distilled off under reduced pressure to obtain 47 g (yield: 99%) of sodium heptadecafluorododecyl glycidyl phosphate.
Workup
- additionwas added
- customto obtain a uniform mixture
- temperatureThereafter, the reaction system was cooled down to 30° C., to which
- customThe resultant NaCl precipitate was removed by filtration
- distillationthe ethanol was distilled off under reduced pressure
Sources & evidence
- ORD record
- ord-10c2833cbf704f35940dbf3346e52ecf
- Source dataset
- uspto-grants-1989_07
- Patent number
- US04845239
Linked notes
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