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Methanol → 1H-Perfluorohexane

HRID 53414
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 53414
CO.C(O)(C)C.[OH-].[K+].[C:9](I)([C:12]([C:15]([C:18]([C:21]([C:24]([F:27])([F:26])[F:25])([F:23])[F:22])([F:20])[F:19])([F:17])[F:16])([F:14])[F:13])([F:11])[F:10]>[Cr].[Co].O>[CH:9]([C:12]([C:15]([C:18]([C:21]([C:24]([F:25])([F:26])[F:27])([F:22])[F:23])([F:19])[F:20])([F:17])[F:16])([F:14])[F:13])([F:11])[F:10]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 887MethanolHCID 3776IsopropanolHCID 14797Potassium HydroxideHCID 677331,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane

Produkt 1

HCID 677301H-PerfluorohexaneAusbeute 92,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 11332432
Hastelloy C
Katalysator
HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
55 °C

Versuchsvorschrift

Into a 20 l Hastelloy C autoclave equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 7700 g of methanol, 60 g of isopropyl alcohol and 1980 g (30 mols) of 85% potassium hydroxide were charged. The reactor was heated to bring the internal temperature to 55° C. Then, 4460 g (10 mols) of C6F13I was fed thereto over a period of two hours. While maintaining the reactor at 55° C. stirring was continued for 10 hours. The conversion was more than 99.9%. Then, 3200 g of water was added to dissolve precipitated potassium iodide. The crude reaction solution was separated into two layers, and the fluorocarbon layer (lower layer) was further washed twice with 3200 g of water to obtain 2951 g of C6F13H (purity: 99.9%, 3.9 ppm of C6F13I was detected). In the reactor, no formation of tar was observed.

Aufarbeitung

  1. temperatureThe reactor was heated
  2. customto 55° C
  3. waitwas continued for 10 hours
  4. dissolutionto dissolve
  5. customprecipitated potassium iodide
  6. customThe crude reaction solution
  7. customwas separated into two layers
  8. washthe fluorocarbon layer (lower layer) was further washed twice with 3200 g of water

Quellen und Nachweise

ORD-Eintrag
ord-54f8a64d08b74411b846a4c35d500602
Quelldatensatz
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05618986

Notizen zur Reaktion

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