Water → C4F9Och2I

HRID 1857898Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1857898
[C:1]([O:14][CH2:15]Cl)([C:4]([C:7]([C:10]([F:13])([F:12])[F:11])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2].[I-:17].[Na+].O>CC(C)=O>[C:1]([O:14][CH2:15][I:17])([C:4]([C:7]([C:10]([F:13])([F:12])[F:11])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2]

Komponenten

5

Versuchsvorschrift

C4F9OCH2Cl (50 g, 0.175 mole, isomer ratio n/i=95:5) was combined with sodium iodide (52.5 g, 0.38 mole) in acetone (200 g) and heated to reflux overnight. Water was added and the acetone distilled from the reaction vessel using a Dean-Stark apparatus. The product was washed with water to remove residual acetone. Glc of the residue (52.6 g) revealed it to be 82.6 wt. % of the desired product C4F9OCH2I, which was further purified by distillation. The distillation fraction boiling at 110-115° C. was found to be 97.8 wt. % of the desired product with a 96/4 normal to iso ratio.

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux overnight
  3. distillationthe acetone distilled from the reaction vessel
  4. washThe product was washed with water
  5. customto remove residual acetone
  6. distillationwas further purified by distillation

Quellen und Nachweise

ORD-Eintrag
ord-0aab472405594b39ab28ef8a173bdefb
Quelldatensatz
uspto-grants-2000_11
Patentnummer
US06149980

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