Potassium Carbonate → 1,1,1,2,4,4,5,5,5-Nonafluoropentane

HRID 427214Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 427214
[F:1][C:2]([F:15])([F:14])[CH:3]([F:13])[CH:4](F)[C:5]([F:11])([F:10])[C:6]([F:9])([F:8])[F:7].C(=O)([O-])[O-].[K+].[K+]>>[F:1][C:2]([F:14])([F:15])[CH:3]([F:13])[CH2:4][C:5]([F:11])([F:10])[C:6]([F:7])([F:9])[F:8]

Komponenten

3

Reaktionsbedingungen

Temperatur
30 °C

Versuchsvorschrift

To 1,1,1,2,3,4,4,5,5,5-decafluoropentane (at a purity of 99.9%, 20 g, 79.4 mmol) was added 100 ml of an aqueous 4M potassium carbonate solution; and the resulting mixture was agitated at 30° C. for 10 hours. The reaction solution was separated into two layers; and the organic layer was again charged, together with 5% palladium carbon (0.55 g) and 0.33 g of tridecane, in a 70-ml autoclave, for hydrogenation at 50 ° C. under a hydrogen pressure of 6 kg/cm2. When hydrogen absorption was ceased 15 hours later, the reaction was terminated; then, the resulting solution was neutralized with saturated sodium bicarbonate solution, followed by distillation, to recover nonafluoropentane (1,1,1,2,4,4,5,5,5- and 1,1,1,3,4,4,5,5,5-nonafluoropentane mixture)(at a total purity of 99.7%; 10.4 g).

Aufarbeitung

  1. customThe reaction solution was separated into two layers
  2. additionand the organic layer was again charged, together with 5% palladium carbon (0.55 g) and 0.33 g of tridecane, in a 70-ml autoclave, for hydrogenation at 50 ° C. under a hydrogen pressure of 6 kg/cm2
  3. customWhen hydrogen absorption
  4. waitwas ceased 15 hours
  5. customlater, the reaction was terminated
  6. distillationfollowed by distillation
  7. customto recover nonafluoropentane (1,1,1,2,4,4,5,5,5- and 1,1,1,3,4,4,5,5,5-nonafluoropentane

Quellen und Nachweise

ORD-Eintrag
ord-3056a328db204fa7904319d8cb81b934
Quelldatensatz
uspto-grants-2001_11
Patentnummer
US06312759B1

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