Sodium hydroxide ethanol → Sodium heptadecafluorodecyl glycidyl phosphate

HRID 231288Notizen

Reaktionsgleichung

[P:1]([O-:37])([O:31][CH2:32][CH:33]([OH:36])[CH2:34]Cl)([O:3][C:4]([F:30])([F:29])[C:5]([F:28])([F:27])[C:6]([F:26])([F:25])[C:7]([F:24])([F:23])[C:8]([F:22])([F:21])[C:9]([F:20])([F:19])[C:10]([F:18])([F:17])[CH2:11][CH2:12][C:13]([F:16])([F:15])[F:14])=[O:2].[Na+:38].C(O)C.[OH-].[Na+]>C(O)C>[P:1]([O-:37])([O:31][CH2:32][CH:33]1[O:36][CH2:34]1)([O:3][C:4]([F:30])([F:29])[C:5]([F:28])([F:27])[C:6]([F:26])([F:25])[C:7]([F:24])([F:23])[C:8]([F:22])([F:21])[C:9]([F:20])([F:19])[C:10]([F:18])([F:17])[CH2:11][CH2:12][C:13]([F:16])([F:15])[F:14])=[O:2].[Na+:38]

Komponenten

Reaktionsbedingungen

Temperatur: 70 °C

Versuchsvorschrift

20 g (0.030 mol) of sodium heptadecafluorodecyl 2-hydroxy-3-chloropropyl phosphate was charged into a reactor, to which 500 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 16.9 g (0.030 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 18.7 g (yield: 99%) of sodium heptadecafluorodecyl glycidyl phosphate.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag: ord-923e3b563f4a4ea88d5eb6abf9de5f4e
Quelldatensatz: uspto-grants-1989_07
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04845239

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