Potassium Hydroxide → 1H-Perfluorohexane

HRID 53418

Reaktionsgleichung

Reaktionsgleichung von HRID 53418
[OH-].[K+].[C:3](I)([C:6]([C:9]([C:12]([C:15]([C:18]([F:21])([F:20])[F:19])([F:17])[F:16])([F:14])[F:13])([F:11])[F:10])([F:8])[F:7])([F:5])[F:4]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C(O)(C)C>[CH:3]([C:6]([C:9]([C:12]([C:15]([C:18]([F:19])([F:20])[F:21])([F:16])[F:17])([F:13])[F:14])([F:11])[F:10])([F:8])[F:7])([F:5])[F:4]

Komponenten

5

Edukt 2

HCID 14797Potassium HydroxideHCID 677331,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane

Produkt 1

HCID 677301H-PerfluorohexaneAusbeute 91,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 74236Tetrabutylammonium BromideKatalysatorHCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

Into a 1 l four-necked flask equipped with a stirrer, a distillation apparatus-equipped reflux condenser, a dropping funnel and a thermometer, 200 cc of isopropyl alcohol, 87.5 g (0.75 mol) of 48% potassium hydroxide and 1 g of tetrabutyl ammonium bromide were charged. The reactor was heated to bring the internal temperature to 60° C. Then, 223 g (0.5 mol) of C6F13I was dropwise added thereto over a period of one hour. After completion of dropwise addition, heating and refluxing were continued for 3 hours. The conversion at that time was 99.9%. A fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor. This recovered liquid was washed five times with 200 g of water, and acetone and isopropyl alcohol were removed. Thus, 146 g of C6F13H having a purity of 99.9%, was obtained.

Aufarbeitung

  1. customInto a 1 l four-necked flask equipped with a stirrer
  2. distillationa distillation
  3. customapparatus-equipped
  4. temperaturereflux condenser, a dropping funnel
  5. temperatureThe reactor was heated
  6. customto 60° C
  7. additionAfter completion of dropwise addition
  8. temperatureheating
  9. temperaturerefluxing
  10. waitwere continued for 3 hours
  11. distillationA fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor
  12. washThis recovered liquid was washed five times with 200 g of water, and acetone and isopropyl alcohol
  13. customwere removed

Quellen und Nachweise

ORD-Eintrag
ord-170786d7e07c432a8a0b319eaf4533a6
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05618986

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