Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane | HCID 67733 | — |
| Katalysator | Tetrabutylphosphonium bromide | HCID 76564 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1H-Perfluorohexane | HCID 67730 | 98,1% |
Reaktionsschritte
Into a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 200 cc of methanol, 74.3 g (1.1 mols) of 85% potassium hydroxide and 1 g of tetrabutylphosphonium 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 the dropwise addition, heating and refluxing were continued for tow hours. The conversion at that time was 98.1%. The heating and refluxing were further continued for two hours. Then, the reactor was cooled to room temperature, and 200 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 with 300 g of water to recover the fluorocarbon. Thus, 157 g of C6F13H having a purity of 99.1%, was obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05618986 |
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| Quelldatensatz | uspto-grants-1997_04 |
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| ORD ID | ord-21a112d1251042d38557af52c999c171 |
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| Quellennotiz | uspto-grants-1997_04 |
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